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Chemistry
Organic Building Blocks
Ketones
acetylacetonate
Vanadyl acetylacetonate
Chemistry
Material Science Catalysts Ligands
Organic Building Blocks
Magnetic Materials Transition metal
Ketones
Magnetic Metal Complexes Vanadium
acetylacetonate

[ CAS No. 3153-26-2 ] {[proInfo.proName]}

,{[proInfo.pro_purity]}
Cat. No.: {[proInfo.prAm]}
Chemical Structure| 3153-26-2
Chemical Structure| 3153-26-2
Structure of 3153-26-2 * Storage: {[proInfo.prStorage]}
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Quality Control of [ 3153-26-2 ]

COA NMR CNMR HPLC LC-MS

Related Doc. of [ 3153-26-2 ]

SDS Specification
Alternatived Products of [ 3153-26-2 ]

Product Details of [ 3153-26-2 ]

CAS No. :3153-26-2 MDL No. :MFCD00000032
Formula : C10H14O5V Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 265.16 Pubchem ID :-
Synonyms :

Calculated chemistry of [ 3153-26-2 ]

Physicochemical Properties

Num. heavy atoms : 15
Num. arom. heavy atoms : 0
Fraction Csp3 : 0.4
Num. rotatable bonds : 0
Num. H-bond acceptors : 4.0
Num. H-bond donors : 0.0
Molar Refractivity : 51.81
TPSA : 52.6 Ų

Pharmacokinetics

GI absorption : High
BBB permeant : Yes
P-gp substrate : No
CYP1A2 inhibitor : No
CYP2C19 inhibitor : No
CYP2C9 inhibitor : No
CYP2D6 inhibitor : No
CYP3A4 inhibitor : No
Log Kp (skin permeation) : -6.95 cm/s

Lipophilicity

Log Po/w (iLOGP) : 0.0
Log Po/w (XLOGP3) : 1.22
Log Po/w (WLOGP) : 1.92
Log Po/w (MLOGP) : -0.65
Log Po/w (SILICOS-IT) : -1.32
Consensus Log Po/w : 0.23

Druglikeness

Lipinski : 0.0
Ghose : None
Veber : 0.0
Egan : 0.0
Muegge : 0.0
Bioavailability Score : 0.56

Water Solubility

Log S (ESOL) : -2.15
Solubility : 1.75 mg/ml ; 0.00702 mol/l
Class : Soluble
Log S (Ali) : -1.92
Solubility : 2.98 mg/ml ; 0.012 mol/l
Class : Very soluble
Log S (SILICOS-IT) : -2.34
Solubility : 1.14 mg/ml ; 0.00456 mol/l
Class : Soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 1.0 alert
Leadlikeness : 1.0
Synthetic accessibility : 4.95

Safety of [ 3153-26-2 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 3153-26-2 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 3153-26-2 ]

[ 3153-26-2 ] Synthesis Path-Downstream   1~88

  • 1
  • [ 3153-26-2 ]
  • [ 1835-65-0 ]
  • vanadyl hexadecafluorophthalocyanine [ No CAS ]
YieldReaction ConditionsOperation in experiment
87.5% With octanol; oxygen; benzonitrile; at 150℃; for 5h;Product distribution / selectivity; Example 6; The reaction was performed by following the procedure of Example 4 while using 11.6 gr (0.0438 mol) of vanadyl acetyl acetonate in place of vanadium trichloride. The conversion of <strong>[1835-65-0]tetrafluorophthalonitrile</strong> was determined by liquid chromatography, to find to be 98.8percent. The reaction slurry resulting from the cyclization was filtered to separate a solid component. The solid component was washed with 300 gr of benzonitrile, then washed with 100 gr of methanol, and dried under a reduced pressure at 150° C. for 12 hours. The weight of the target product, hexadecafluorovanadylphthalocyanine, as calculated from the weight after drying, was 28.4 gr (yield: 87.5 mol percent).
Reference： [1]Patent: US2005/203293,2005,A1 .Location in patent: Page/Page column 17
  • 2
  • [ 3153-26-2 ]
  • H2Pc(dib)4(OBu)8 [ No CAS ]
  • C119H110N8O9V [ No CAS ]
YieldReaction ConditionsOperation in experiment
76% With tributyl-amine In N,N-dimethyl-formamide Heating / reflux; 2 Example 2; (b) Vanadyl octabutoxyphthalocyanine; IRB001 PCTH2Pc(dib)4(OBu)s (113 mg; 0.071 mmol) was suspended in dry DMF (5 mL) and then vanadyl acetylacetonate (97 mg; 0.37 mmol) and tributylamine (500 uL) were added consecutively with stirring. The resulting mixture was heated under reflux overnight, cooled and diluted with dichloromethane (200 mL). The solution was washed with water (100 mL), HC1 (0.1 M; 2 x 100 mL) and saturated NaHC03 (100 mL), and dried (MgS04). Removal of the solvent left a dark green solid that was dissolved in toluene and purified by column chromatography on neutral alumina (toluene). The first green band contained the product and removal of the solvent afforded a green powder (90 mg; 76%). JH NMR (CDC13) (all signals are broad) 81.15-1.26; 1.67-1.76; 2.1-2.4; 4.9-5.0; 6.4-6.7; 7.10-7.23; 7.64-7.70; K** 768 (5.2), 688 (4.6), 401 (4.6), 357 (4.6), 331 (4.7) nm.
Reference： [1]Current Patent Assignee: BASF SE - WO2006/15407, 2006, A1 Location in patent: Page/Page column 46-47
  • 3
  • [ 3153-26-2 ]
  • [ 918663-88-4 ]
  • vanadyl tetrakis[6,7-di(4'-methoxyphenoxy)]naphthalocyanine [ No CAS ]
YieldReaction ConditionsOperation in experiment
84% With 1,8-diazabicyclo[5.4.0]undec-7-ene In pentan-1-ol Heating / reflux; 3 Example 3Vanadyl tetrakis[6,7-(4'-methoxyphenoxy)]naphthalocyanine (7); IRB014-PCT EPO A mixture of the dinitrile 4 (213 mg, 0.503 mmol), vanadyl acetylacetonate (45 mg, 0.169 mmol) and DBU (130 μL, 130 mg, 0.854 mmol) in 1-pentanol (2 mL) was heated at reflux overnight. The reaction mixture was cooled to room temperature and diluted with methanol (20 mL). The resulting solid was filtered off and washed with methanol, water and acetone to give 7 as a dark reddish-brown powder (185 mg, 84%).UV-Vis-NIR (DMSO, 10.8 μM): 808 nm (ε = 84,000); 718 (ε = 19,500).
Reference： [1]Current Patent Assignee: BASF SE - WO2007/2980, 2007, A1 Location in patent: Page/Page column 41-42
  • 4
  • [ 3153-26-2 ]
  • bismuth (III) nitrate pentahydrate [ No CAS ]
  • bismuth vanadate [ No CAS ]
YieldReaction ConditionsOperation in experiment
In acetic acid; pentane-2,4-dione Bi(NO3)3 in AcOH, bis(acetylacetonato)oxovanadium(IV) in acetylacetone mixed in 1:1 stoich. ratio; spin coated onto glass; fired at ca 500°C for 30 min; repeated 6 times;
With air In acetic acid; acetylacetone metal-organic decomposition method (Sayama et al., Chem. Commun. 2003, 2908 and Galembeck et al., Thin Solid Films 2000, 365, 90): Bi(NO3)3 in acetic acid and VO(acac)2 in acetyl acetone spin coated on FTO glass, fired at 500 °C in air for 30 min;
Stage #1: bis(acetylacetonate)oxovanadium; bismuth (III) nitrate pentahydrate With acetic acid In ethanol; N,N-dimethyl-formamide at 20℃; Stage #2: at 400 - 550℃; for 1h; Calcination;
Stage #1: bismuth (III) nitrate pentahydrate With p-benzoquinone ethanol; potassium iodide for 0.333333h; Stage #2: bis(acetylacetonate)oxovanadium In dimethyl sulfoxide at 450℃; for 1h;
Stage #1: bismuth (III) nitrate pentahydrate With LACTIC ACID; nitric acid; p-benzoquinone; potassium iodide In ethanol; water Electrochemical reaction; Stage #2: bis(acetylacetonate)oxovanadium In dimethyl sulfoxide at 450℃; for 2h;
Stage #1: bismuth (III) nitrate pentahydrate With nitric acid; p-benzoquinone; potassium iodide In ethanol; water at 20℃; for 0.0833333h; Stage #2: bis(acetylacetonate)oxovanadium at 450℃; for 2h;

Reference： [1]Sayama, Kazuhiro; Wang, Nini; Miseki, Yugo; Kusama, Hitoshi; Onozawa-Komatsuzaki, Nobuko; Sugihara, Hideki [Chemistry Letters, 2010, vol. 39, # 1, p. 17 - 19]
[2]Sayama, Kazuhiro; Nomura, Atsushi; Arai, Takeo; Sugita, Tsuyoshi; Abe, Ryu; Yanagida, Masatoshi; Oi, Takashi; Iwasaki, Yasukazu; Abe, Yoshimoto; Sugihara, Hideki [Journal of Physical Chemistry B, 2006, vol. 110, # 23, p. 11352 - 11360]
[3]Cheng, Yongliang; Chen, Jiangtao; Yan, Xingbin; Zheng, Zongmin; Xue, Qunji [RSC Advances, 2013, vol. 3, # 43, p. 20606 - 20612]
[4]Wang, Jing-Hao; Li, Xu-Bing; Li, Jian; Lei, Tao; Wu, Hao-Lin; Nan, Xiao-Lei; Tung, Chen-Ho; Wu, Li-Zhu [Chemical Communications, 2019, vol. 55, # 70, p. 10376 - 10379]
[5]Chen, Tao; Chen, Yihuang; He, Bing; Hu, Xiaoqin; Huang, Jing; Li, Zhen; Liu, Xueqin; Wang, Yang; Yi, Ping; Zhao, Mingyang [Journal of Materials Chemistry A, 2020, vol. 8, # 31, p. 15976 - 15983]
[6]Gao, Rui-Ting; He, Jinlu; Liu, Xianhu; Nakajima, Tomohiko; Sun, Mao; Wang, Lei; Zhang, Xueyuan [Angewandte Chemie - International Edition, 2021, vol. 60, # 32, p. 17601 - 17607][Angew. Chem., 2021, vol. 133, # 32, p. 17742 - 17748]
  • 5
  • [ 3153-26-2 ]
  • [ 3946-91-6 ]
  • N,N′-bis(salicylidene)-o-phenylenediamine vanadium(IV) oxide complex [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% In ethanol; at 20℃; for 24h; General procedure: VO(acac)2 was added carefully in small portionsto a suspension of the appropriate ligand (1-5) in anhydrous ethanol(50 mL) in a 1:1.1 molar ratio. An excess of ligand in each reaction wasused to ensure its maximum complexation. Reactions were magneticstirred for 24 h at RT in a 100 mL flat-bottomed flask. Reaction mediacolor changed from the ligand suspension color (yellow or orange) togreen (6-8) or khaki (9-10). The change of color was very fast in allcases yielding a turbid reaction media. The solid products formed werefiltered off, purified with cold anhydrous ethanol (3×10 mL) washesand vacuum-dried. Thereafter, vanadium complexes (6-10) were driedat 100 C for 24 h. Solubility data indicate the amount of vanadiumcoordination compound in mg dissolved in a specific volume in μL ofDMSO. Sonication was sometimes used to promote an effective dissolutionof the complexes. 2.5.2.1. N,N′-bis(salicylidene)-o-phenylenediamine vanadium(IV) oxidecomplex (6). Reagents: VO(acac)2 (0.713 g, 2.7 mmol) and 1 (0.951 g,3.0 mmol). Product: 0.980 g (2.57 mmol) of a green powder wasobtained after purification. Yield: 95%. Mp > 300 C. Solubility:soluble 1 in 100 parts of DMSO at 25 C. Anal. Calcd. for VO(C20H14N2O2) (M=381.3 gmol-1): C, 63.00; H, 3.70; N, 7.35%.Found: C, 62.84; H, 3.39; N, 7.49%. IR (ATR, υ cm-1): 3048(CeH)arom, 1601 (C]N), 1577, 1531, 1459 (C]C)arom, 1190 (CeO),981 (V]O). μeff 0.87 BM. TOF+, m/z calcd. For (M+H)+: 382.3.Found: 382.1. UV/Vis (DMSO) λ (nm): 317, 399. Crystals wereobtained by vapor diffusion in acetone as solvent and ethanol asprecipitant at RT.
Reference： [1]Inorganica Chimica Acta,2018,vol. 480,p. 197 - 206
[2]Inorganic Chemistry,2006,vol. 45,p. 5924 - 5937
  • 6
  • [ 3153-26-2 ]
  • [ 94-91-7 ]
  • [ 29876-29-7 ]
Reference： [1]Polyhedron,1997,vol. 16,p. 1517 - 1528
  • 7
  • [ 89-73-6 ]
  • [ 3153-26-2 ]
  • [ 121437-23-8 ]
Reference： [1]Inorganica Chimica Acta,1989,vol. 155,p. 171 - 174
  • 8
  • [ 3153-26-2 ]
  • [ 1198-55-6 ]
  • [ 143493-60-1 ]
YieldReaction ConditionsOperation in experiment
95% With 2,2'-bipyridine In tetrahydrofuran stirring for several h; filtered; elem. anal.;
Reference： [1]Simpson, Cathy L.; Pierpont, Cortlandt G. [Inorganic Chemistry, 1992, vol. 31, # 21, p. 4308 - 4313]
  • 9
  • [ 940-07-8 ]
  • [ 3153-26-2 ]
  • {VO(pyrazine-2,6-dicarboxylate)(H2O)2}*2H2O [ No CAS ]
Reference： [1]Zeitschrift fur Anorganische und Allgemeine Chemie,
    Zeitschrift fuer Anorganische und Allgemeine Chemie,1985,vol. 524,p. 40 - 50
  • 10
  • [ 3153-26-2 ]
  • [ 2050-14-8 ]
  • [ 150153-53-0 ]
Reference： [1]Inorganic Chemistry,1993,vol. 32,p. 4249 - 4255
  • 11
  • [ 3153-26-2 ]
  • [ 2050-14-8 ]
  • {(azobenzene-2,2'-diolate)(O)VOV(O)(azobenzene-2,2'-diolate)} [ No CAS ]
Reference： [1]Journal of the Chemical Society, Dalton Transactions,1993,p. 2857 - 2858
  • 12
  • [ 3153-26-2 ]
  • [ 2050-14-8 ]
  • potassium (2,2'-dihydroxyazobenzenato)dioxovanadate(V)*1.5H2O [ No CAS ]
Reference： [1]Inorganic Chemistry,1993,vol. 32,p. 5343 - 5348
  • 13
  • [ 3153-26-2 ]
  • [ 19485-38-2 ]
  • VO(H2O)(C5H7O2)(C6H5N2O4) [ No CAS ]
Reference： [1]Journal of the American Chemical Society,2000,vol. 122,p. 767 - 775
  • 14
  • [ 3153-26-2 ]
  • [ 140-07-8 ]
  • [VO(acetylacetonate)]2(C10H20N2O4) [ No CAS ]
Reference： [1]European Journal of Inorganic Chemistry,1998,p. 799 - 805
  • 15
  • [ 3153-26-2 ]
  • [ 151433-25-9 ]
  • (O)V(S,S)-N,N'-bis-(3,5-di-tert-butylsalicylidene)-1,2-cyclohexenediamine-2H) [ No CAS ]
Reference： [1]Journal of the Chemical Society, Dalton Transactions,1996,p. 1229 - 1236
  • 16
  • [ 3153-26-2 ]
  • [ 1596-64-1 ]
  • [ 95-01-2 ]
  • VO(2+)*OC6H3(OH)CHNCH(CH2C3H3N2)CH2O(2-)*C2H5OH=[VO(OC6H3(OH)CHNCH(CH2C3H3N2)CH2O)(C2H5OH)] [ No CAS ]
Reference： [1]Inorganica Chimica Acta,2004,vol. 357,p. 2237 - 2244
  • 17
  • [ 3153-26-2 ]
  • [ 90-02-8 ]
  • [ 1596-64-1 ]
  • VO(2+)*OC6H4CHNCH(CH2C3H3N2)CH2O(2-)*C2H5OH=[VO(OC6H4CHNCH(CH2C3H3N2)CH2O)(C2H5OH)] [ No CAS ]
Reference： [1]Inorganica Chimica Acta,2004,vol. 357,p. 2237 - 2244
  • 18
  • [ 3153-26-2 ]
  • [ 80937-33-3 ]
  • [ 5993-91-9 ]
  • [VO2(acac-ambmz)] [ No CAS ]
Reference： [1]Inorganic Chemistry,2006,vol. 45,p. 5924 - 5937
  • 19
  • [ 3153-26-2 ]
  • [ 131380-91-1 ]
  • [VO(C12H14NO2)2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
70% In toluene (argon); reflux (24 h); solvent removal (vac., 120°C), recrystn. (EtOH); elem. anal.;
Reference： [1]Bolm, Carsten; Luongb, Thi Kirn Khanh; Harms, Klaus [Chemische Berichte, 1997, vol. 130, # 7, p. 887 - 890]
  • 20
  • [ 3153-26-2 ]
  • [ 22107-30-8 ]
  • (2-hydroxyacetophenone semicarbazone)dioxovanadium(IV) [ No CAS ]
YieldReaction ConditionsOperation in experiment
100% In dichloromethane soln. of semicarbazone in CH2Cl2 added to soln. of V compd. in CH2Cl2; stored at room temp. for 24 h;
41% In methanol soln. of semicarbazone in CH3OH added to soln. of V compd. in CH3OH; mixt. stirred for 20 min; concd.; stored at room temp. for 24 h; crystals filtered off; dried under vac.; elem. anal.;
Reference： [1]Maia, Pedro Ivo Da S.; Deflon, Victor M.; De Sousa, Gerimario F.; Lemos, Sebastiao S.; Batista, Alzir A.; Nascimento, Otaciro R.; Niquet, Elke [Zeitschrift fur Anorganische und Allgemeine Chemie, 2007, vol. 633, # 5-6, p. 783 - 789]
[2]Maia, Pedro Ivo Da S.; Deflon, Victor M.; De Sousa, Gerimario F.; Lemos, Sebastiao S.; Batista, Alzir A.; Nascimento, Otaciro R.; Niquet, Elke [Zeitschrift fur Anorganische und Allgemeine Chemie, 2007, vol. 633, # 5-6, p. 783 - 789]
  • 21
  • [ 3153-26-2 ]
  • [ 22107-30-8 ]
  • [ 1012049-50-1 ]
YieldReaction ConditionsOperation in experiment
38% In acetonitrile soln. of semicarbazone in CH3CN added to soln. of V compd. in CH3CN; mixt. stirred for 10 min; volume reduced to half under vac.; ppt. filtered off; washed with small amt. of n-hexane; dried under vac.; elem. anal.;
Reference： [1]Maia, Pedro Ivo Da S.; Deflon, Victor M.; De Sousa, Gerimario F.; Lemos, Sebastiao S.; Batista, Alzir A.; Nascimento, Otaciro R.; Niquet, Elke [Zeitschrift fur Anorganische und Allgemeine Chemie, 2007, vol. 633, # 5-6, p. 783 - 789]
  • 22
  • [ 3153-26-2 ]
  • [ 22107-30-8 ]
  • (2-oxyacetophenone semicarbazone)dioxovanadium(V) [ No CAS ]
YieldReaction ConditionsOperation in experiment
68% In methanol soln. of V compd. and semicarbazone in CH3OH stirred at room temp. for 3d; solid filtered off; washed with small amt. of n-hexane; dried under vac.; recrystd. from CH3OH; mixt. of monomer and dimer; elem. anal.;
Reference： [1]Maia, Pedro Ivo Da S.; Deflon, Victor M.; De Sousa, Gerimario F.; Lemos, Sebastiao S.; Batista, Alzir A.; Nascimento, Otaciro R.; Niquet, Elke [Zeitschrift fur Anorganische und Allgemeine Chemie, 2007, vol. 633, # 5-6, p. 783 - 789]
  • 23
  • [ 3153-26-2 ]
  • [ 835-64-3 ]
  • [ 1221404-81-4 ]
YieldReaction ConditionsOperation in experiment
82% In tetrahydrofuran; at 20℃;Inert atmosphere; Reflux; To a stirred solution of vanadyl acetylacetonate (3.13g, 11.80 mmol) in THF (30 ml_), was added a suspension of <strong>[835-64-3]2-(2-hydroxyphenyl)benzoxazole</strong> (5.00 g, 23.67 mmol) in THF (30 ml_) under nitrogen atmosphere. A brown suspension was observed after a few minutes of stirring, which was refluxed for 6 hours and stirred over the weekend at room temperature. The brown solid was filtered off, washed thoroughly with THF and dried in vacuum oven at 8O0C for 8 hours giving 4.7 g of product (82% yield). Sublimation (25O0C1 10'6 Torr.) yielded an analytical sample (3.9 g from 4.7 g); melting point at N/AC (DSC peak).
Reference： [1]Inorganica Chimica Acta,2010,vol. 363,p. 807 - 812
[2]Patent: WO2010/20352,2010,A1 .Location in patent: Page/Page column 58-59
  • 24
  • [ 3153-26-2 ]
  • [ 3411-95-8 ]
  • [ 11060-63-2 ]
YieldReaction ConditionsOperation in experiment
78% In tetrahydrofuran at 20℃; Inert atmosphere; Reflux; 20 To a stirred solution of vanadyl acetylacetonate (2.91 g, 10.97 mmol) in THF (30 mL), was added a suspension of 2-(2- hydroxyphenyl)benzothiazole (5.00 g, 22.00 mmol) in THF (30 mL) under nitrogen atmosphere. A brown suspension was observed after a few minutes of stirring, which was refluxed for 6 hours and stirred over the weekend at room temperature. The brown solid was filtered off, washed thoroughly with THF and dried in vacuum oven at 800C for 8 hours giving 3.1 g of product (78% yield). Sublimation (25O0C, 10~6 Torr.) yielded an analytical sample (2.6 g from 3.1 g); melting point at 4020C (DSC peak).
Reference： [1]Current Patent Assignee: MERCK KGAA - WO2010/20352, 2010, A1 Location in patent: Page/Page column 59
  • 25
  • [ 288-32-4 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 7732-18-5 ]
  • [ 80937-33-3 ]
  • [(imidazole)O2V(μ-N.N'-bis(diacetyl)hydrazine(-2H))VO2(imidazole)]*2H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
41% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:2 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 26
  • [ 288-13-1 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 80937-33-3 ]
  • [(pyrazole)O2V(μ-N.N'-bis(diacetyl)hydrazine(-2H))VO2(pyrazole)] [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:2 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 27
  • [ 288-13-1 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 80937-33-3 ]
  • [(acetylacetone)2OV(μ-O)VO(pyrazole)(μ-N.N'-bis(diacetyl)hydrazine(-2H))(pyrazole)OV(μ-O)VO(acetylacetone)2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
26% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:4 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 28
  • [ 288-32-4 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 80937-33-3 ]
  • [(acetylacetone)2OV(μ-O)VO(imidazole)(μ-N.N'-bis(diacetyl)hydrazine(-2H))(imidazole)OV(μ-O)VO(acetylacetone)2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
31% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:4 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 29
  • [ 67-51-6 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 80937-33-3 ]
  • [(3,5-dimethylpyrazole)O2V(μ-N.N'-bis(diacetyl)hydrazine(-2H))VO2(3,5-dimethylpyrazole)] [ No CAS ]
YieldReaction ConditionsOperation in experiment
47% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:2 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 30
  • [ 67-51-6 ]
  • [ 3153-26-2 ]
  • [ 3148-73-0 ]
  • [ 80937-33-3 ]
  • [(acetylacetone)2OV(μ-O)VO(3,5-dimethylpyrazole)(μ-N.N'-bis(diacetyl)hydrazine(-2H))(pyrazole)OV(μ-O)VO(acetylacetone... [ No CAS ]
YieldReaction ConditionsOperation in experiment
32% In water; acetonitrile aq. soln. of H2diah added to MeCN soln. of Himdz and V compd. (1:2:4 molaer ratio), mixt. refluxed for 6 h; filtered, crystd. on storage at 5°c for 7 d, ppt. filtered off, washed (MeCN), dried in air, elem. anal.;
Reference： [1]Sarkar, Anindita; Pal, Samudranil [European Journal of Inorganic Chemistry, 2009, # 35, p. 5391 - 5398]
  • 31
  • [ 3153-26-2 ]
  • [ 1761-56-4 ]
  • [(μ-oxo)bis(oxovanadium(V)(salicylideneaminophenol(-2H)))] [ No CAS ]
Reference： [1]Inorganica Chimica Acta,2010,vol. 364,p. 144 - 149
  • 32
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • [ 15006-57-2 ]
YieldReaction ConditionsOperation in experiment
96% In acetone at 20℃; Synthesis of (HQ)2VIV(O) (10)Complex 10 has been reported previously, and was prepared according to a modified version of a published procedure (Pasquali, M.; Landi, A.; Floriani, C. Inorg. Chem. 1979, 18, 2397-2400). In a vial, VIV(O)(acac)2 (155 mg, 0.583 mmol) and 8-hydroxyquinoline (174 mg, 1.20 mmol) were suspended in acetone. The reaction mixture was stirred at room temperature overnight, affording a yellow suspension. The yellow solid was collected on a frit, washed with diethyl ether (1×1 mL) and dried under vacuum. Yield: 198 mg (96%). The IR spectrum of the product matched reported data for 10 (Pasquali, M.; Landi, A.; Floriani, C. Inorg. Chem. 1979, 18, 2397-2400).
In toluene Inert atmosphere; Schlenk technique;
In dichloromethane at 30℃; for 2h;
Reference： [1]Current Patent Assignee: TRIAD NATIONAL SECURITY LLC - US2012/232279, 2012, A1 Location in patent: Page/Page column 8
[2]Tuskaev, Vladislav A.; Kolosov, Nikolay A.; Kurmaev, Dmitrii A.; Gagieva, Svetlana C.; Khrustalev, Victor N.; Ikonnikov, Nikolay S.; Efimov, Nikolay N.; Ugolkova, Elena A.; Minin, Vadim V.; Bulychev, Boris M. [Journal of Organometallic Chemistry, 2015, vol. 798, p. 393 - 400]
[3]She, Jialuo; Lin, Xiangfeng; Fu, Zaihui; Li, Jianwei; Tang, Senpei; Lei, Ming; Zhang, Xin; Zhang, Chao; Yin, Dulin [Catalysis science and technology, 2019, vol. 9, # 2, p. 275 - 285]
  • 33
  • [ 3153-26-2 ]
  • [ 87578-89-0 ]
  • 3,4-bis((E)-2-hydroxybenzylideneamino)benzoic acid oxovanadium [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% In methanol at 50℃; for 3h; Synthesis of vanadyl Schiff base complexes The complexes were prepared by the reaction of Schiff base ligands with vanadyl acetylacetonate in methanol. To a methanolic solution (50 ml) of vanadyl acetylacetonate (1 mmol, 0.267 gr) was added to the ligand (1 mmol in 30 ml methanol) and the mixture was stirred for 3 h at 50 C. The resulting precipitate was collected by filtration, washed with H2O and dried in vacuum (Scheme 2- sup). 3,4-bis((E)-2-hydroxybenzylideneamino)benzoic acid oxovanadium(IV), [VOL1] Color: black green; yield: 60%, m.p.: >250 °C. FT-IR (KBr, cm-1): 2400-3700(νO-H(acid)), 1607(νC=O), 1580(νC=N), 1440, 1465(νC=C), 1200(νC-O), 975(νV=O), 555(νC-N-M), 450(νC-O-M). UV-Vis: (λmax, nm, MeOH): 273, 404. Mass spectra (ESI): m/z(%) = 425 [M]+, 381, 303, and 99.
Reference： [1]Mohammadi, Khosro; Niad, Mahmood; Irandoost, Amene [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2013, vol. 107, p. 145 - 150]
  • 34
  • [ 3153-26-2 ]
  • [ 1428859-23-7 ]
  • 3,4-bis((E)-2-hydroxy-3-methoxybenzylideneamino)benzoic acid oxovanadium [ No CAS ]
YieldReaction ConditionsOperation in experiment
65% In methanol at 50℃; for 3h; Synthesis of vanadyl Schiff base complexes The complexes were prepared by the reaction of Schiff base ligands with vanadyl acetylacetonate in methanol. To a methanolic solution (50 ml) of vanadyl acetylacetonate (1 mmol, 0.267 gr) was added to the ligand (1 mmol in 30 ml methanol) and the mixture was stirred for 3 h at 50 C. The resulting precipitate was collected by filtration, washed with H2O and dried in vacuum (Scheme 2- sup). 3,4-bis((E)-2-hydroxy-3-methoxybenzylideneamino)benzoic acid oxovanadium(IV), [VOL2] Color: green; yield: 65%, m.p.: >250 °C. FT-IR (KBr, cm-1): 2400-3700(νO-H(acid)), 1680(νC-O), 1600(νC-N), 1480, 1540(νC-C), 1250(νC-O), 978(νV-O), 550(νC-N-M), 450(νC-O-M). UV-Vis: (λmax, nm, MeOH): 305, 374. Mass spectra (ESI): m/z(%) = 485 [M]+, 425, 381, 303, and 99.
Reference： [1]Mohammadi, Khosro; Niad, Mahmood; Irandoost, Amene [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2013, vol. 107, p. 145 - 150]
  • 35
  • [ 3153-26-2 ]
  • [ 1428859-24-8 ]
  • 3,4-bis((E)-2,4-dihydroxybenzylideneamino)benzoic acidoxovanadium [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% In methanol at 50℃; for 3h; Synthesis of vanadyl Schiff base complexes The complexes were prepared by the reaction of Schiff base ligands with vanadyl acetylacetonate in methanol. To a methanolic solution (50 ml) of vanadyl acetylacetonate (1 mmol, 0.267 gr) was added to the ligand (1 mmol in 30 ml methanol) and the mixture was stirred for 3 h at 50 C. The resulting precipitate was collected by filtration, washed with H2O and dried in vacuum (Scheme 2- sup). 3,4-bis((E)-2,4-dihydroxybenzylideneamino)benzoic acid)oxovanadium(IV), [VOL3] Color: green; yield: 60%, m.p.: >250 °C. FT-IR (KBr, cm-1): 2400-3700(νO-H(acid)), 1610(νC-O), 1600(νC-N), 1460, 1490(νC-C), 1250(νC-O), 990 (νV-O), 530(νC-N-M), 460(νC-O-M). UV-Vis: (λmax, nm, MeOH): 262, 345. Mass spectra (ESI): m/z(%) = 457 [M]+, 413, 335, and 99.
Reference： [1]Mohammadi, Khosro; Niad, Mahmood; Irandoost, Amene [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2013, vol. 107, p. 145 - 150]
  • 36
  • [ 3153-26-2 ]
  • [ 144-62-7 ]
  • [ 172606-22-3 ]
  • C6H4O16V2*2H2O*C18H22N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
33% In ethanol at 20℃; for 4h;
Reference： [1]Chen, Chen; Bai, Feng-Ying; Zhang, Rui; Song, Ge; Shan, Hui; Xing, Na; Xing, Yong-Heng [Journal of Coordination Chemistry, 2013, vol. 66, # 4, p. 671 - 688]
  • 37
  • [ 3153-26-2 ]
  • sodium perchlorate [ No CAS ]
  • [ 26082-96-2 ]
  • [oxovanadium(IV)(bis-(2-pyridylmethyl)benzylamine)(acetylacetonate)](perchlorate) [ No CAS ]
YieldReaction ConditionsOperation in experiment
80% In methanol at 25℃; for 3h; Inert atmosphere; Schlenk technique; General procedure: Complexes [VO(Fc-pic)(acac)](ClO4) (1) and [VO(Ph-pic)(acac)](ClO4) (3) were prepared by a general synthetic procedure in which an equimolar mixture of VO(acac)2, the respective tridentate ligand Fc-pic (0.39g, 1.0mmol) for 1 and Ph-pic (0.29g, 1.0mmol) for 3, and an excess of sodium perchlorate were taken in 30ml methanol. The solution was stirred at room temperature for 3h to get a green solution. It was filtered and the solution on slow evaporation gave a green solid which was washed with cold methanol and diethyl ether, and finally dried in vacuo over P4O10 [Yield: ∼80%].
Reference： [1]Balaji, Babu; Somyajit, Kumar; Banik, Bhabatosh; Nagaraju, Ganesh; Chakravarty, Akhil R. [Inorganica Chimica Acta, 2013, vol. 400, p. 142 - 150]
  • 38
  • [ 3153-26-2 ]
  • [ 439556-66-8 ]
  • sodium perchlorate [ No CAS ]
  • [oxovanadium(IV)(ferrocenylmethylbis-(2-pyridylmethylamine))(acetylacetonate)](perchlorate) [ No CAS ]
YieldReaction ConditionsOperation in experiment
82% In methanol at 25℃; for 3h; Inert atmosphere; Schlenk technique; General procedure: Complexes [VO(Fc-pic)(acac)](ClO4) (1) and [VO(Ph-pic)(acac)](ClO4) (3) were prepared by a general synthetic procedure in which an equimolar mixture of VO(acac)2, the respective tridentate ligand Fc-pic (0.39g, 1.0mmol) for 1 and Ph-pic (0.29g, 1.0mmol) for 3, and an excess of sodium perchlorate were taken in 30ml methanol. The solution was stirred at room temperature for 3h to get a green solution. It was filtered and the solution on slow evaporation gave a green solid which was washed with cold methanol and diethyl ether, and finally dried in vacuo over P4O10 [Yield: ∼80%].
Reference： [1]Balaji, Babu; Somyajit, Kumar; Banik, Bhabatosh; Nagaraju, Ganesh; Chakravarty, Akhil R. [Inorganica Chimica Acta, 2013, vol. 400, p. 142 - 150]
  • 39
  • [ 3153-26-2 ]
  • [ 804517-57-5 ]
  • [(oxovanadium(V)(2-[((2-hydroxypropan-2-yl)(pyridin-2-ylmethyl)amino)methyl]phenol(-3H)))2O] [ No CAS ]
YieldReaction ConditionsOperation in experiment
74% With air In acetonitrile at 60 - 70℃; for 2.5h; Reflux; 2.5.1 [V2o3(L1)2] (1) To a stirred solution of [VO(acac)2] (93 mg, 0.35 mmol), in 20 mL acetonitrile was added H2L1 ligand (100 mg, 0.35 mmol). The reaction mixture was then stirred for half an hour at room temperature and then it was warmed gently on a water bath for 2 h. On slow evaporation of the solvent a dark violet colored mass was obtained. The product on recrystallization from dichloromethane-hexane afforded violet colored crystals. Yield: 186 mg (74%). Elemental Anal. Calc. for C34H40N4O7V2: C, 56.83; H, 5.61; N, 7.80. Found: C, 57.06; H, 5.68; N, 7.91%. IR (KBr, cm-1): ν(V=O) 978; ν(V-O-V) 860. UV-Vis [CH2Cl2; λmax, nm (ε, M-1 cm-1)]: 505 (2763), 408 (3625), 263 (22022). 1H NMRexptl {300 MHz, CDCl3, δ (ppm), J (Hz)}: 9.30 (H13, d, J = 5.9), 7.87 (H11, t, J = 6.9), 7.44 (H10, t, J = 6.6), 7.26 (H12, m), 6.64-9.30 (8H, ArH), 4.05 (2 H8, s), 3.85 (2 H7, s), 3.75 (2 H14, s), 1.43 (-CH3, s), 1.23 (-CH3, s). 1H NMRtheor {δ (ppm)}: 9.50 (H13), 7.35 (H11), 6.90 (H12), 6.52 (H10), 5.95-9.50 (8H, ArH), 4.18 (H7), 3.87 (H8), 3.73 (H14), 0.98 (-CH3), 0.68 (-CH3). Epc (VV/VIV): -0.38 V (irr).
Reference： [1]Mondal, Pallab; Hens, Amar; Rajak, Kajal Krishna [Polyhedron, 2013, vol. 54, p. 228 - 236]
  • 40
  • [ 3153-26-2 ]
  • 2-[((1-hydroxy-2-methylpropyl)(pyridin-2-ylmethyl)amino)methyl]phenol [ No CAS ]
  • [(oxovanadium(V)(2-[((1-hydroxy-2-methylpropyl)(pyridin-2-ylmethyl)amino)methyl]phenol(-3H)))2O] [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% With air In acetonitrile at 60 - 70℃; for 2.5h; Reflux; 2.5.2 [V2o3(L2)2] (2) General procedure: To a stirred solution of [VO(acac)2] (93 mg, 0.35 mmol), in 20 mL acetonitrile was added H2L1 ligand (100 mg, 0.35 mmol). The reaction mixture was then stirred for half an hour at room temperature and then it was warmed gently on a water bath for 2 h. On slow evaporation of the solvent a dark violet colored mass was obtained. The product on recrystallization from dichloromethane-hexane afforded violet colored crystals.
Reference： [1]Mondal, Pallab; Hens, Amar; Rajak, Kajal Krishna [Polyhedron, 2013, vol. 54, p. 228 - 236]
  • 41
  • [ 3153-26-2 ]
  • 2-[((1-hydroxy-3-methylbutyl)(pyridin-2-ylmethyl)amino)methyl]phenol [ No CAS ]
  • [(oxovanadium(V)(2-[((1-hydroxy-3-methylbutyl)(pyridin-2-ylmethyl)amino)methyl]phenol(-3H)))2O] [ No CAS ]
YieldReaction ConditionsOperation in experiment
76% With air In acetonitrile at 60 - 70℃; for 2.5h; Reflux; 2.5.3 [V2o3(L3)2] (3) General procedure: To a stirred solution of [VO(acac)2] (93 mg, 0.35 mmol), in 20 mL acetonitrile was added H2L1 ligand (100 mg, 0.35 mmol). The reaction mixture was then stirred for half an hour at room temperature and then it was warmed gently on a water bath for 2 h. On slow evaporation of the solvent a dark violet colored mass was obtained. The product on recrystallization from dichloromethane-hexane afforded violet colored crystals.
Reference： [1]Mondal, Pallab; Hens, Amar; Rajak, Kajal Krishna [Polyhedron, 2013, vol. 54, p. 228 - 236]
  • 42
  • [ 28384-96-5 ]
  • [ 3153-26-2 ]
  • [ 121-44-8 ]
  • C30H21N3O15V(2-)*2C6H16N(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
In methanol at 20℃; for 24h;
Reference： [1]Baramov, Todor; Keijzer, Karlijn; Irran, Elisabeth; Moesker, Eva; Baik, Mu-Hyun; Suessmuth, Roderich [Chemistry - A European Journal, 2013, vol. 19, # 32, p. 10536 - 10542]
  • 43
  • [ 3153-26-2 ]
  • [ 1266680-11-8 ]
  • C24H32Br2N4O6V2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
61% In methanol at 20℃; for 0.5h; Synthesis of the Complex [VO2L2]2 (2) General procedure: methanol solution (5 mL) ofVO(acac)2 (0.1 mmol, 26.5 mg) was added to a methanol solution (10 mL)of HL1 (0.1 mmol, 25.1 mg) under stirring. The mixture was stirred at roomtemperature for 30 min to give a yellow solution. The resulting solution wasallowed to stand in air for a few days. Yellow block-shaped crystals suitable for X-ray single crystal diffraction were formed at the bottom of the vessel. Theisolated product was washed with cold methanol, and dried in air.
Reference： [1]Hu, Hua-Nan; Liu, Shi-Yong; Ma, Yu-Ping [Journal of the Chilean Chemical Society, 2013, vol. 58, # 2, p. 1695 - 1697]
  • 44
  • [ 19535-47-8 ]
  • [ 3153-26-2 ]
  • [ 387846-36-8 ]
  • C28H21N7O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
75% In ethanol; for 3.5h;Inert atmosphere; Reflux; General procedure: The new [VIVO(L-2H)(NN)] complexes, where L = L3-L5 andNN = bipy or dppz, were synthesized by the following procedure:0.375 mmol of L (78 mg L3, 84 mg L4 or 108 mg L5) and 0.375 mmolof NN (59 mg bipy or 110 mg dppz) were suspended in 15 mL of absolute alcohol previously purged with nitrogen for 10 min. [VIVO(acac)2](0.375 mmol, 100 mg) was suspended in 6 mL of absolute alcohol,previously purged with nitrogen, and was added to the previous mixture. This was then heated at reflux under nitrogen for 3.5 h.The brown-red solid formed was filtered off from the hot mixture, and then washed three times with 2 mL portions of EtOH:Et2O(1:1).
Reference： [1]Journal of Inorganic Biochemistry,2013,vol. 127,p. 150 - 160
  • 45
  • [ 19535-47-8 ]
  • [ 3153-26-2 ]
  • [ 215459-02-2 ]
  • C27H18BrN7O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
74% In ethanol; for 3.5h;Inert atmosphere; Reflux; General procedure: The new [VIVO(L-2H)(NN)] complexes, where L = L3-L5 andNN = bipy or dppz, were synthesized by the following procedure:0.375 mmol of L (78 mg L3, 84 mg L4 or 108 mg L5) and 0.375 mmolof NN (59 mg bipy or 110 mg dppz) were suspended in 15 mL of absolute alcohol previously purged with nitrogen for 10 min. [VIVO(acac)2](0.375 mmol, 100 mg) was suspended in 6 mL of absolute alcohol,previously purged with nitrogen, and was added to the previous mixture. This was then heated at reflux under nitrogen for 3.5 h.The brown-red solid formed was filtered off from the hot mixture, and then washed three times with 2 mL portions of EtOH:Et2O(1:1).
Reference： [1]Journal of Inorganic Biochemistry,2013,vol. 127,p. 150 - 160
  • 46
  • [ 3153-26-2 ]
  • [ 387846-36-8 ]
  • C10H12N3O5V [ No CAS ]
YieldReaction ConditionsOperation in experiment
82% In ethanol at 20℃; Reflux; Syntheses of the dioxidovanadium(V) complexes, [VVO2(L-H)], 1-3 General procedure: The new [VVO2(L-H)] complexes, where L = 2-hydroxy-3-methoxybenzaldehyde semicarbazone (L3), 3-ethoxysalicylaldehydesemicarbazone (L4) or 5-bromo-2-hydroxy-3-methoxybenzaldehydesemicarbazone (L5), were prepared by first mixing [VIVO(acac)2](100 mg, 0.375 mmol, acac = acetylacetonate) with L (0.375 mmol)in ethanol (10 mL) and then keeping for 24 h under reflux. The reaction mixture was then stirred during 5-10 days at room temperature. In each case a yellowsolidwas isolated by centrifugation and recrystallizedfrom boiling ethanol.
Reference： [1]Fernández, Mariana; Becco, Lorena; Correia, Isabel; Benítez, Julio; Piro, Oscar E.; Echeverria, Gustavo A.; Medeiros, Andrea; Comini, Marcelo; Lavaggi, María Laura; González, Mercedes; Cerecetto, Hugo; Moreno, Virtudes; Pessoa, Joao Costa; Garat, Beatriz; Gambino, Dinorah [Journal of Inorganic Biochemistry, 2013, vol. 127, p. 150 - 160]
  • 47
  • [ 3153-26-2 ]
  • [ 10534-59-5 ]
  • C16H36N(1+)*5V(5+)*13O(2-)*C2H3O2(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine In acetonitrile at 20℃; for 6h; 4.1. Synthesis of polyoxovanadates General procedure: Preparation of four different solutions of tetradecavanadates, VxOyALz (A = Cl- or CH3CO2-, L = (C2H5)4N+ or (C4H9)4N+), was carried out according to a modified literature procedure [31]. All chemicals were purchased from Sigma-Aldrich and used as received. Briefly, 1.5 mmol of vanadyl acetylacetonate [VO(acac)2] and 0.6 mmol of either tetraethylammonium chloride [(C2H5)4NCl], tetrabutylammonium chloride [(C4H9)4NCl], tetraethylammonium acetate [(C2H5)4N(CH3CO2)] or tetrabutylammonium acetate [(C4H9)4N(CH3CO2)] were dissolved in 50 mL of acetonitrile. 0.8 mmol of triethyl amine was then added to the initial mixtures while stirring constantly at room temperature. Following 6 h of reaction, an Oakton 10 series pH meter (calibrated using buffers of pH 4, 7 and 10 at room temperature) was used to determine the pH of the resulting brown-colored solutions. The product mixtures were de-solvated under reduced pressure using a VWR1400E vacuum oven. Recrystallization was carried out in approximately 3 mL of N,N-dimethylformamide (N,N-DMF) by heating the solution to the boiling temperature (153 °C) for 10 min. Any remaining N,N-DMF was then evaporated in vacuum to obtain pure dry crystals of polyoxovanadates. A small quantity of crystals was dissolved in acetonitrile to prepare concentrated stock solutions. These stock solutions were diluted further by factors of ten or one hundred in acetonitrile prior to analysis by ESI-MS.
Reference： [1]Johnson, Grant E.; Al Hasan, Naila M.; Laskin, Julia [International Journal of Mass Spectrometry, 2013, vol. 354-355, p. 333 - 341]
  • 48
  • [ 3153-26-2 ]
  • [ 10534-59-5 ]
  • C16H36N(1+)*7V(5+)*18O(2-)*C2H3O2(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine In acetonitrile at 20℃; for 6h; 4.1. Synthesis of polyoxovanadates General procedure: Preparation of four different solutions of tetradecavanadates, VxOyALz (A = Cl- or CH3CO2-, L = (C2H5)4N+ or (C4H9)4N+), was carried out according to a modified literature procedure [31]. All chemicals were purchased from Sigma-Aldrich and used as received. Briefly, 1.5 mmol of vanadyl acetylacetonate [VO(acac)2] and 0.6 mmol of either tetraethylammonium chloride [(C2H5)4NCl], tetrabutylammonium chloride [(C4H9)4NCl], tetraethylammonium acetate [(C2H5)4N(CH3CO2)] or tetrabutylammonium acetate [(C4H9)4N(CH3CO2)] were dissolved in 50 mL of acetonitrile. 0.8 mmol of triethyl amine was then added to the initial mixtures while stirring constantly at room temperature. Following 6 h of reaction, an Oakton 10 series pH meter (calibrated using buffers of pH 4, 7 and 10 at room temperature) was used to determine the pH of the resulting brown-colored solutions. The product mixtures were de-solvated under reduced pressure using a VWR1400E vacuum oven. Recrystallization was carried out in approximately 3 mL of N,N-dimethylformamide (N,N-DMF) by heating the solution to the boiling temperature (153 °C) for 10 min. Any remaining N,N-DMF was then evaporated in vacuum to obtain pure dry crystals of polyoxovanadates. A small quantity of crystals was dissolved in acetonitrile to prepare concentrated stock solutions. These stock solutions were diluted further by factors of ten or one hundred in acetonitrile prior to analysis by ESI-MS.
Reference： [1]Johnson, Grant E.; Al Hasan, Naila M.; Laskin, Julia [International Journal of Mass Spectrometry, 2013, vol. 354-355, p. 333 - 341]
  • 49
  • [ 3153-26-2 ]
  • [ 56-34-8 ]
  • C8H20N(1+)*14V(5+)*34O(2-)*Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine; In acetonitrile; at 20℃; for 6h; General procedure: Preparation of four different solutions of tetradecavanadates, VxOyALz (A = Cl- or CH3CO2-, L = (C2H5)4N+ or (C4H9)4N+), was carried out according to a modified literature procedure [31]. All chemicals were purchased from Sigma-Aldrich and used as received. Briefly, 1.5 mmol of vanadyl acetylacetonate [VO(acac)2] and 0.6 mmol of either <strong>[56-34-8]tetraethylammonium chloride</strong> [(C2H5)4NCl], tetrabutylammonium chloride [(C4H9)4NCl], tetraethylammonium acetate [(C2H5)4N(CH3CO2)] or tetrabutylammonium acetate [(C4H9)4N(CH3CO2)] were dissolved in 50 mL of acetonitrile. 0.8 mmol of triethyl amine was then added to the initial mixtures while stirring constantly at room temperature. Following 6 h of reaction, an Oakton 10 series pH meter (calibrated using buffers of pH 4, 7 and 10 at room temperature) was used to determine the pH of the resulting brown-colored solutions. The product mixtures were de-solvated under reduced pressure using a VWR1400E vacuum oven. Recrystallization was carried out in approximately 3 mL of N,N-dimethylformamide (N,N-DMF) by heating the solution to the boiling temperature (153 C) for 10 min. Any remaining N,N-DMF was then evaporated in vacuum to obtain pure dry crystals of polyoxovanadates. A small quantity of crystals was dissolved in acetonitrile to prepare concentrated stock solutions. These stock solutions were diluted further by factors of ten or one hundred in acetonitrile prior to analysis by ESI-MS.
Reference： [1]International Journal of Mass Spectrometry,2013,vol. 354-355,p. 333 - 341
  • 50
  • [ 3153-26-2 ]
  • [ 56-34-8 ]
  • 2C8H20N(1+)*14V(5+)*34O(2-)*Cl(1-)*HO(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine; In acetonitrile; at 20℃; for 6h; General procedure: Preparation of four different solutions of tetradecavanadates, VxOyALz (A = Cl- or CH3CO2-, L = (C2H5)4N+ or (C4H9)4N+), was carried out according to a modified literature procedure [31]. All chemicals were purchased from Sigma-Aldrich and used as received. Briefly, 1.5 mmol of vanadyl acetylacetonate [VO(acac)2] and 0.6 mmol of either <strong>[56-34-8]tetraethylammonium chloride</strong> [(C2H5)4NCl], tetrabutylammonium chloride [(C4H9)4NCl], tetraethylammonium acetate [(C2H5)4N(CH3CO2)] or tetrabutylammonium acetate [(C4H9)4N(CH3CO2)] were dissolved in 50 mL of acetonitrile. 0.8 mmol of triethyl amine was then added to the initial mixtures while stirring constantly at room temperature. Following 6 h of reaction, an Oakton 10 series pH meter (calibrated using buffers of pH 4, 7 and 10 at room temperature) was used to determine the pH of the resulting brown-colored solutions. The product mixtures were de-solvated under reduced pressure using a VWR1400E vacuum oven. Recrystallization was carried out in approximately 3 mL of N,N-dimethylformamide (N,N-DMF) by heating the solution to the boiling temperature (153 C) for 10 min. Any remaining N,N-DMF was then evaporated in vacuum to obtain pure dry crystals of polyoxovanadates. A small quantity of crystals was dissolved in acetonitrile to prepare concentrated stock solutions. These stock solutions were diluted further by factors of ten or one hundred in acetonitrile prior to analysis by ESI-MS.
Reference： [1]International Journal of Mass Spectrometry,2013,vol. 354-355,p. 333 - 341
  • 51
  • [ 3153-26-2 ]
  • [ 1112-67-0 ]
  • C16H36N(1+)*14V(5+)*34O(2-)*Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With triethylamine In acetonitrile at 20℃; for 6h; 4.1. Synthesis of polyoxovanadates General procedure: Preparation of four different solutions of tetradecavanadates, VxOyALz (A = Cl- or CH3CO2-, L = (C2H5)4N+ or (C4H9)4N+), was carried out according to a modified literature procedure [31]. All chemicals were purchased from Sigma-Aldrich and used as received. Briefly, 1.5 mmol of vanadyl acetylacetonate [VO(acac)2] and 0.6 mmol of either tetraethylammonium chloride [(C2H5)4NCl], tetrabutylammonium chloride [(C4H9)4NCl], tetraethylammonium acetate [(C2H5)4N(CH3CO2)] or tetrabutylammonium acetate [(C4H9)4N(CH3CO2)] were dissolved in 50 mL of acetonitrile. 0.8 mmol of triethyl amine was then added to the initial mixtures while stirring constantly at room temperature. Following 6 h of reaction, an Oakton 10 series pH meter (calibrated using buffers of pH 4, 7 and 10 at room temperature) was used to determine the pH of the resulting brown-colored solutions. The product mixtures were de-solvated under reduced pressure using a VWR1400E vacuum oven. Recrystallization was carried out in approximately 3 mL of N,N-dimethylformamide (N,N-DMF) by heating the solution to the boiling temperature (153 °C) for 10 min. Any remaining N,N-DMF was then evaporated in vacuum to obtain pure dry crystals of polyoxovanadates. A small quantity of crystals was dissolved in acetonitrile to prepare concentrated stock solutions. These stock solutions were diluted further by factors of ten or one hundred in acetonitrile prior to analysis by ESI-MS.
Reference： [1]Johnson, Grant E.; Al Hasan, Naila M.; Laskin, Julia [International Journal of Mass Spectrometry, 2013, vol. 354-355, p. 333 - 341]
  • 52
  • [ 67-56-1 ]
  • [ 3153-26-2 ]
  • bis((3-hydroxy-5-(hydroxymethyl)-2-methylpyridin-4-yl)methylene)succinohydrazide dihydrochloride [ No CAS ]
  • [(VO)2((bis((3-hydroxy-5-(hydroxymethyl)-2-methylpyridin-4-yl)methylene)succinohydrazide)-4H+)(MeO)2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
94% With triethylamine at 60℃; for 3.5h; Inert atmosphere; 2.2.4. [(VO)2(H10pyr2sucdihyd-4H+)(MeO)2] The ligand H10pyr2sucdihyd (0.2 mmol, 0.104 g) was dissolved in8 ml of methanol and mixed with 0.2 mmol (0.052 mg) of 98% vanadyl(IV) acetylacetonate and 200 lL of Et3N. The mixture was stirred for 3.5 h at 60 °C. The few precipitate was removed by filtration and after 3 days the solvent evaporation (under normal conditions of temperature and pressure) yielded deep red crystals. Yield: 94%.
Reference： [1]Back, Davi Fernando; Manzoni De Oliveira, Gelson; Roman, Daiane; Ballin, Marco Aurélio; Kober, Roger; Piquini, Paulo Cesar [Inorganica Chimica Acta, 2014, vol. 412, p. 6 - 14]
  • 53
  • [ 3153-26-2 ]
  • 7-amino-4-methyl-5-aza-3-hepten-2-one [ No CAS ]
  • VO(7-amino-5-aza-4-methylhept-3-en-2-one)(acac) [ No CAS ]
YieldReaction ConditionsOperation in experiment
65.5% In ethanol for 5h; Reflux; 4 Oxovanadium(IV) complexes General procedure: complexesA hot solution of VO(acac)2(0.265 g, 0.001 mol) in ethanol(10 ml) was added dropwise to ethanolic solution (10 ml) of theappropriate ligand (HL1or HL2) (0.001 mol). The reaction mixturewas heated and stirred under reflux for 5 h. The complex slowlyseparated out from filtered, and the solid was washed with hotwater followed by ethanol and dried at 100C. Recrystallizationfrom MeCN gave analytically pure products
Reference： [1]Von Willingh, Gavin; Abbo, Hanna S.; Titinchi, Salam J.J. [Catalysis Today, 2014, vol. 227, p. 96 - 104]
  • 54
  • [ 3153-26-2 ]
  • [ 495-18-1 ]
  • N'-(3,5-dibromo-2-hydroxybenzylidene)nicotinohydrazide [ No CAS ]
  • C20H13Br2N4O5V [ No CAS ]
YieldReaction ConditionsOperation in experiment
67% In methanol at 20℃; for 1h; [VOL1L] (1) General procedure: A methanolic solution (15 mL) of VO(acac)2 (0.26 g, 1.0 mM) was added to a methanolic solution (15 mL) of H2L1 (0.43 g, 1.0 mM) and benzohydroxamic acid (0.14 g, 1.0 mM). The mixture was stirred at room temperature for 1 h to give a brown solution. Single crystals of the complex, suitable for X-ray diffraction, were formed at the bottom of the vessel on slow evaporation of the solution in air for a few days.
Reference： [1]Li, An-Mei [Journal of Coordination Chemistry, 2014, vol. 67, # 12, p. 2076 - 2085]
  • 55
  • [ 3153-26-2 ]
  • [ 1445781-32-7 ]
  • (2-[(2-isopropylaminoethylimino)methyl]-6-methylphenolato)dioxovanadium(V) [ No CAS ]
YieldReaction ConditionsOperation in experiment
71% In methanol at 20℃; for 0.5h; 2.3. Synthesis of the complexes General procedure: A methanolic solution (20 cm3) of the Schiff base (0.5 mmol) was added with stirring to amethanolic solution (20 cm3) of VO(acac)2 (0.5mmol, 0.133 g). The mixtures were stirredat room temperature for 30 min to give yellow solutions. X-ray quality single crystals wereformed by slow evaporation of the solutions in air after a few days.
Reference： [1]Qian, Shao-Song; You, Zhong-Lu; Li, Ying-Nan; Hu, Xue; Zhang, Mei; Zhu, Hai-Liang [Journal of Coordination Chemistry, 2013, vol. 66, # 8, p. 1311 - 1319]
  • 56
  • [ 3153-26-2 ]
  • [ 1204685-62-0 ]
  • bis(5-methoxy-2-[(pyridin-2-ylmethylimino)methyl]phenolato)dioxovanadium(V) [ No CAS ]
YieldReaction ConditionsOperation in experiment
56% In methanol at 20℃; for 0.5h; 2.3. Synthesis of the complexes General procedure: A methanolic solution (20 cm3) of the Schiff base (0.5 mmol) was added with stirring to amethanolic solution (20 cm3) of VO(acac)2 (0.5mmol, 0.133 g). The mixtures were stirredat room temperature for 30 min to give yellow solutions. X-ray quality single crystals wereformed by slow evaporation of the solutions in air after a few days.
Reference： [1]Qian, Shao-Song; You, Zhong-Lu; Li, Ying-Nan; Hu, Xue; Zhang, Mei; Zhu, Hai-Liang [Journal of Coordination Chemistry, 2013, vol. 66, # 8, p. 1311 - 1319]
  • 57
  • [ 89-73-6 ]
  • [ 3153-26-2 ]
  • N’-(2-hydroxy-5-methylbenzylidene)-4-hydroxybenzohydrazide [ No CAS ]
  • [ 7732-18-5 ]
  • [VO(N’-(2-hydroxy-5-methylbenzylidene)-4-hydroxybenzohydrazide(-2H))(salicylohydroxamate)]*3H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% In ethanol;Reflux; H2La (0.2 mmol, 61.2 mg), benzohydroxamic acid (0.2 mmol, 27.4 mg) and VO(acac)2 (0.2 mmol, 53.0 mg) were mixed and added to methanol (20 mL), and the mixture was boiled under refluxed until the color of the solution turned to deep brown. Block-shaped single crystals of the complex were obtained by slow evaporation of the solutionin air. The crystals were isolated by suction filtration,washed successively with cold ethanol and diethylether, and then air dried. Yield: 55%. Analysis: Found: C 58.8%, H 4.3%, N 7.5%. Calculated for C27H24N3O7V: C58.6%, H 4.4%, N 7.6%. Selected IR data (nu/cm-1, KBr):3430 (nuO-H); 3232 (nuN-H); 1602 (nuC=N); 975 (nuV=O).
Reference： [1]Acta Chimica Slovenica,2014,vol. 61,p. 629 - 636
  • 58
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • [ 108-95-2 ]
  • C24H17N2O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
85.7% In acetonitrile at 20℃; for 6h; 1 Production Example 1 Synthesis of Vanadium Complex of Formula (2a-1) Production Example 1 Synthesis of Vanadium Complex of Formula (2a-1) [0061] Bis(acetylacetonato)oxovanadium (IV) (182 mg, 0.69 mmol) was suspended in acetonitrile (5 mL) followed bythe addition of 8-quinolinol (199 mg, 1.37 mmol) and phenol (5 mL). After stirring this for 6 hours at room temperature,the solvent was distilled off under reduced pressure. After adding diisopropyl ether (10 mL) to the residue, the precipitatedcrystals were filtered and washed with diisopropyl ether (5 mL). The resulting wet crystals were dried for 7 hours at 40°Cto obtain a vanadium complex of the aforementioned formula (2a-1) (264 mg, yield: 85.7%).[0062] 1H-NMR(400MHz, CDCl3) δ8.64(d, 1H, J=4.4Hz), 8.49(d, 1H, J=3.2Hz), 8.15(d, 1H, J=7.2Hz), 8.04(d, 1H,J=7.2Hz), 7.54-7.60(m, 2H), 7.27-7.31 (m, 6H), 7.17-7.23(m, 4H), 6.95-6.99(m, 1H)
Reference： [1]Current Patent Assignee: SAGAMI CHEMICAL RESEARCH INSTITUTE; MANAC INCORPORATED - EP2799419, 2014, A1 Location in patent: Paragraph 0060; 0061; 0062
  • 59
  • [ 148-24-3 ]
  • [ 112-92-5 ]
  • [ 3153-26-2 ]
  • C36H49N2O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
66.4% In acetonitrile at 20℃; for 5h; 2 Production Example 2 Synthesis of Vanadium Complex of Formula (2a-2) Production Example 2 Synthesis of Vanadium Complex of Formula (2a-2) [0064] Bis(acetylacetonato)oxovanadium (IV) (182 mg, 0.69 mmol) was suspended in acetonitrile (5 mL) followed bythe addition of 8-quinolinol (199 mg, 1.37 mmol) and 1-octadecanol (370 mg, 1.37 mmol). After stirring this for 5 hoursat room temperature, the precipitated crystals were filtered and washed with acetonitrile (5 mL). After suspending theresulting wet crystals in tetrahydrofuran (5 mL) and stirring for 1 hour at room temperature, the crystals were filtered andwashed with tetrahydrofuran (5 mL). The resulting wet crystals were dried for 16 hours at 40°C to obtain a vanadiumcomplex of the aforementioned formula (2a-2) (285 mg, yield: 66.4%).[0065] 1H-NMR(400MHz, CDCl3) δ(ppm): 8.61(d, 1H, J=4.8Hz), 8.47(d, 1H, J=4.4Hz), 8.11(d, 1H, J=8.3Hz), 8.03(d,1H, J=8.2Hz), 7.52(t, 2H, J=7.8Hz), 7.14-7.25(m, 6H), 6.03(dt, 1H, J=6.5, 11.1Hz), 5.63(dt, 1H, J=6.5, 11.1Hz), 1.85(t,2H, 6.5Hz), 1.16-1.43(m, 30H), 0.88(t, 3H, J=7.0Hz)
Reference： [1]Current Patent Assignee: SAGAMI CHEMICAL RESEARCH INSTITUTE; MANAC INCORPORATED - EP2799419, 2014, A1 Location in patent: Paragraph 0063; 0064; 0065
  • 60
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • [ 40716-66-3 ]
  • C33H37N2O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
58.6% In acetonitrile at 20℃; for 5h; 4 Production Example 4 Synthesis of Vanadium Complex of Formula (2a-4) Production Example 4 Synthesis of Vanadium Complex of Formula (2a-4) [0070] Bis(acetylacetonato)oxovanadium (IV) (182 mg, 0.69 mmol) was suspended in acetonitrile (5 mL) followed bythe addition of 8-quinolinol (199 mg, 1.37 mmol) and (E)-nerolidol (305 mg, 1.37 mmol). After stirring this for 5 hours atroom temperature, diisopropyl ether (5 mL) was injected. The precipitated crystals were filtered and washed with diisopropylether (5 mL). The resulting wet crystals were dried for 6 hours at 40°C under reduced pressure to obtain avanadium complex of the aforementioned formula (2a-4) (232 mg, yield: 58.6%).
Reference： [1]Current Patent Assignee: SAGAMI CHEMICAL RESEARCH INSTITUTE; MANAC INCORPORATED - EP2799419, 2014, A1 Location in patent: Paragraph 0069; 0070
  • 61
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • [ 108-93-0 ]
  • C24H23N2O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% In acetonitrile at 20℃; for 20h; 12 Production Example 12 Synthesis of Vanadium Complex of Formula (2a-12) Production Example 12[0091]Synthesis of Vanadium Complex of Formula (2a-12) [0092] Bis(acetylacetonato)oxovanadium (IV) (182 mg, 0.69 mmol) was suspended in acetonitrile (5 mL) followed bythe addition of 8-quinolinol (199 mg, 1.37 mmol) and cyclohexanol (5 mL). After stirring this for 20 hours at roomtemperature, the solvent was distilled off under reduced pressure. After adding diisopropyl ether (10 mL) to the residue,the precipitate that formed was filtered and the resulting solid was washed with diisopropyl ether followed by dryingunder reduced pressure to obtain a vanadium complex of the aforementioned formula (2a-12) (266 mg, yield: 85%).[0093] 1H-NMR(400MHz, CDCl3) δ(ppm): 8.61(d, 1H, J=3.9Hz), 8.46(d, 1H, J=3.9Hz), 8.10(d, 1H, J=8.4Hz), 8.03(d,1H, J=8.4Hz), 7.54(m, 2H), 7.14-7.31(m, 6H), 6.04(m, 1H), 2.30(m, 2H), 1.29-1.78(m, 7H), 1.14(m,lH)
Reference： [1]Current Patent Assignee: SAGAMI CHEMICAL RESEARCH INSTITUTE; MANAC INCORPORATED - EP2799419, 2014, A1 Location in patent: Paragraph 0091; 0092; 0093
  • 62
  • [ 3153-26-2 ]
  • [ 27895-70-1 ]
  • C20H20N2O3V [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% Stage #1: N-CH2CHCH2-salicylideneimine With triethylamine In methanol for 0.166667h; Stage #2: bis(acetylacetonate)oxovanadium In methanol at 25℃; for 12h; Preparation of complexes General procedure: General synthesisA MeOH or CHCl3 solution (20 cm3) of allylamine (IUPAC name:3-amino-prop-1-ene) (3 mmol) was added dropwise to a MeOH orCHCl3 solution (20 cm3) of the salicylaldehyde (IUPAC name:2-hydroxybenzaldehyde) (3 mmol). The yellow, air stable solutionwas stirred for 2 h in ambient temperature. Then a solution of triethylamine(4 mmol) in absolute MeOH (5 cm3) was added to thesolution. The solution was essentially dark yellow at this time.The mixture stirred for 10 min, and then a solution of appropriatemetal salt (1.5 mmol Zn(NO3)26H2O, CuCl22H2O and VO(acac)2salts and 1 mmol for CoCl26H2O salt) in absolute MeOH (20 cm3)was added dropwise. The resulting solution was stirred for 12 hambient temperature.Vanadium(II) complex VOL2The resultant clear yellow solution was allowed to stand overnight.After concentration at room temperature, dark yellow precipitatewas collected by filtration. Appropriate single crystals forX-ray crystallography were obtained directly from the reactionmixture. The typical yield was 72%. Anal. calc. for C20H20N2O3V:C: 62.02, H: 5.20, N: 7.23. Found: C: 61.87, H: 5.26, N: 7.24.Selected IR data (KBr, cm1): 1622 (mCN), 1473 (mCAN), 1328 (mCAO).
Reference： [1]Khorshidifard, Mahsa; Amiri Rudbari, Hadi; Kazemi-Delikani, Zahra; Mirkhani, Valiollah; Azadbakht, Reza [Journal of Molecular Structure, 2015, vol. 1081, p. 494 - 505]
  • 63
  • [ 3153-26-2 ]
  • 2-[(2-ethylaminoethylimino)methyl]-6-methylphenol [ No CAS ]
  • [VO2(2-[(2-ethylaminoethylimino)methyl]-6-methylphenol)]2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
73% Stage #1: bis(acetylacetonate)oxovanadium; 2-[(2-ethylaminoethylimino)methyl]-6-methylphenol In methanol for 0.5h; Reflux; Stage #2: With air In methanol at 20℃; Synthesis of the Complex The Schiff base (0.5 mmol, 0.10 g) in methanol (20 mL) was added with stirring to VO(acac)2 (0.5 mmol, 0.13 mg) in methanol (10 mL). The mixtures were stirred and refluxed for 30 min to give yellow solution. The solution was left stillat room temperature in air to give yellow block-shaped single crystals, which were collected by filtration and dried in vacuum containing anhydrous CaCl2. The yield was 73%.Found: C, 49.87; H, 6.03; N, 9.61; V, 17.82%,C24H34N4O6V2 Anal Calcd.: C, 50.00; H, 5.95; N, 9.72; V,17.67%.
Reference： [1]Zhao, Xiao-Jun; Peng, Qi; Xue, Ling-Wei [Synthesis and Reactivity in Inorganic, Metal-Organic and Nano-Metal Chemistry, 2015, vol. 45, # 11, p. 1674 - 1677]
  • 64
  • [ 3153-26-2 ]
  • [ 731794-67-5 ]
  • C18H22N8O7S2V2(2+)*2Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% In ethanol for 4h; Reflux; Synthesis of μ-oxido bis oxidovanadium complexes General procedure: A mixture of [VO(acac)2] (0.05 g, 0.2 mmol) and the appropriateligand (H2L1, H2L1·HCl, H2L2, H2L2·HCl) (0.2 mmol) in the appro-priate alcohol (20 mL) was refluxed for four hours. The precipitate formed during the reaction was filtered, washed with alcohol, anddried. For all 1H NMR spectra, the pyridoxal CH3 resonance, whichshould appear around 2.5 ppm, was not visible because of overlapwith the DMSO signal.
Reference： [1]Pisk, Jana; Daran, Jean-Claude; Poli, Rinaldo; Agustin, Dominique [Journal of Molecular Catalysis A: Chemical, 2015, vol. 403, p. 52 - 63]
  • 65
  • [ 3153-26-2 ]
  • [ 737-86-0 ]
  • [VO2(Hpydx-inh)] [ No CAS ]
YieldReaction ConditionsOperation in experiment
41% In methanol for 4h; Reflux; Synthesis of dioxidovanadium complexes General procedure: A mixture of [VO(acac)2] (0.05 g, 0.2 mmol) and the appropriateligand (0.2 mmol) in methanol (20 mL) was refluxed for 4 h and the precipitate formed during the reaction was filtered, washed withmethanol and dried.
Reference： [1]Pisk, Jana; Daran, Jean-Claude; Poli, Rinaldo; Agustin, Dominique [Journal of Molecular Catalysis A: Chemical, 2015, vol. 403, p. 52 - 63]
  • 66
  • [ 7791-07-3 ]
  • [ 3153-26-2 ]
  • (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,3-diamine [ No CAS ]
  • (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,3-diamineoxovanadium(IV) perchlorate [ No CAS ]
YieldReaction ConditionsOperation in experiment
55% Stage #1: bis(acetylacetonate)oxovanadium; (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,3-diamine In methanol; N,N-dimethyl-formamide at 60℃; Stage #2: sodium perchlorate monohydrate In methanol; N,N-dimethyl-formamide at 60℃; for 24h; The preparation of oxovanadium(IV) complexes General procedure: The oxovanadium(IV) complexes were prepared by a generalprocedure: 0.1 mmol of each of the ligands (about 0.06 g) was dissolvedin 5 mL of DMF. A methanolic solution (25 mL) ofoxovanadium(IV) acetylacetonate (0.026 g, 0.1 mmol) was addedto above solution and the reaction mixture refluxed for 48-72 h.Then a methanolic solution of sodium perchlorate monohydrate(0.028 g, 0.2 mmol) was added to above solution (10 mL) and thereaction mixture refluxed for 24 h. The solution was concentratedby rotary under vacuum for 6 h. To the concentrated solution, distilledwater was added and the solution stirred to obtain a darkgreenprecipitate. The products were filtered off, then washed withn-hexan and ethylacetate and dried.
Reference： [1]Mohammadi, Khosro; Azad, Seyyedeh Sedigheh; Amoozegar, Ameneh [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2015, vol. 146, p. 221 - 227]
  • 67
  • [ 7791-07-3 ]
  • [ 3153-26-2 ]
  • (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)-2,2-dimethyl-propan-1,3-diamine [ No CAS ]
  • (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)-2,2-dimethylpropane-1,3-diamineoxovanadium(IV) perchlorate [ No CAS ]
YieldReaction ConditionsOperation in experiment
52% Stage #1: bis(acetylacetonate)oxovanadium; (N1E,N3E)-N1,N3-bis(2-amino-3,5-dibromobenzaldehyde)-2,2-dimethyl-propan-1,3-diamine In methanol; N,N-dimethyl-formamide at 60℃; Stage #2: sodium perchlorate monohydrate In methanol; N,N-dimethyl-formamide at 60℃; for 24h; The preparation of oxovanadium(IV) complexes General procedure: The oxovanadium(IV) complexes were prepared by a generalprocedure: 0.1 mmol of each of the ligands (about 0.06 g) was dissolvedin 5 mL of DMF. A methanolic solution (25 mL) ofoxovanadium(IV) acetylacetonate (0.026 g, 0.1 mmol) was addedto above solution and the reaction mixture refluxed for 48-72 h.Then a methanolic solution of sodium perchlorate monohydrate(0.028 g, 0.2 mmol) was added to above solution (10 mL) and thereaction mixture refluxed for 24 h. The solution was concentratedby rotary under vacuum for 6 h. To the concentrated solution, distilledwater was added and the solution stirred to obtain a darkgreenprecipitate. The products were filtered off, then washed withn-hexan and ethylacetate and dried.
Reference： [1]Mohammadi, Khosro; Azad, Seyyedeh Sedigheh; Amoozegar, Ameneh [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2015, vol. 146, p. 221 - 227]
  • 68
  • [ 7791-07-3 ]
  • [ 3153-26-2 ]
  • (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,2-diamine [ No CAS ]
  • (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,2-diamineoxovanadium(IV) perchlorate [ No CAS ]
YieldReaction ConditionsOperation in experiment
56% Stage #1: bis(acetylacetonate)oxovanadium; (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)propan-1,2-diamine In methanol; N,N-dimethyl-formamide at 60℃; Stage #2: sodium perchlorate monohydrate In methanol; N,N-dimethyl-formamide at 60℃; for 24h; The preparation of oxovanadium(IV) complexes General procedure: The oxovanadium(IV) complexes were prepared by a generalprocedure: 0.1 mmol of each of the ligands (about 0.06 g) was dissolvedin 5 mL of DMF. A methanolic solution (25 mL) ofoxovanadium(IV) acetylacetonate (0.026 g, 0.1 mmol) was addedto above solution and the reaction mixture refluxed for 48-72 h.Then a methanolic solution of sodium perchlorate monohydrate(0.028 g, 0.2 mmol) was added to above solution (10 mL) and thereaction mixture refluxed for 24 h. The solution was concentratedby rotary under vacuum for 6 h. To the concentrated solution, distilledwater was added and the solution stirred to obtain a darkgreenprecipitate. The products were filtered off, then washed withn-hexan and ethylacetate and dried.
Reference： [1]Mohammadi, Khosro; Azad, Seyyedeh Sedigheh; Amoozegar, Ameneh [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2015, vol. 146, p. 221 - 227]
  • 69
  • [ 7791-07-3 ]
  • [ 3153-26-2 ]
  • (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)ethane-1,2-diamine [ No CAS ]
  • (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)ethane-1,2-diamineoxovanadium(IV) perchlorate [ No CAS ]
YieldReaction ConditionsOperation in experiment
54% Stage #1: bis(acetylacetonate)oxovanadium; (N1E,N2E)-N1,N2-bis(2-amino-3,5-dibromobenzaldehyde)ethane-1,2-diamine In methanol; N,N-dimethyl-formamide at 60℃; Stage #2: sodium perchlorate monohydrate In methanol; N,N-dimethyl-formamide at 60℃; for 24h; The preparation of oxovanadium(IV) complexes General procedure: The oxovanadium(IV) complexes were prepared by a generalprocedure: 0.1 mmol of each of the ligands (about 0.06 g) was dissolvedin 5 mL of DMF. A methanolic solution (25 mL) ofoxovanadium(IV) acetylacetonate (0.026 g, 0.1 mmol) was addedto above solution and the reaction mixture refluxed for 48-72 h.Then a methanolic solution of sodium perchlorate monohydrate(0.028 g, 0.2 mmol) was added to above solution (10 mL) and thereaction mixture refluxed for 24 h. The solution was concentratedby rotary under vacuum for 6 h. To the concentrated solution, distilledwater was added and the solution stirred to obtain a darkgreenprecipitate. The products were filtered off, then washed withn-hexan and ethylacetate and dried.
Reference： [1]Mohammadi, Khosro; Azad, Seyyedeh Sedigheh; Amoozegar, Ameneh [Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2015, vol. 146, p. 221 - 227]
  • 70
  • [ 3153-26-2 ]
  • C14H17BrN2O2 [ No CAS ]
  • C14H15BrN2O3V [ No CAS ]
YieldReaction ConditionsOperation in experiment
79% In methanol at 50℃; for 1h; Synthesis of the VOL 1.2 mmol of the H2L was dissolved in a 50 mL of absolute methanol and a solution of 1.2 mmol of VO(acac)2 in 50 mL of absolute methanol was added. The resulting solution was heated for 1 h at 50 8C. After evaporating the solvent, the green precipitate was dried in air (Yield 0.37 g, 79%).
Reference： [1]Grivani, Gholamhossein; Ghavami, Abbase; Eigner, Václav; Dušek, Michal; Khalaji, Aliakbar Dehno [Chinese Chemical Letters, 2015, vol. 26, # 6, p. 779 - 784]
  • 71
  • [ 3153-26-2 ]
  • [ 139-13-9 ]
  • [ 5144-89-8 ]
  • 1,10-phenathrolin-1-ium aqua-(nitrilotriacetato-N,O,O',O'')-oxidovanadium(IV) semihydrate [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: bis(acetylacetonate)oxovanadium; nitrilotriacetic acid In water; acetylacetone for 0.5h; Reflux; Stage #2: 1,10-phenanthroline hydrate In methanol at 20℃; 2 Reagents 2.2 The synthesis of (phenH)[VO(NTA)(H2O)]∙1/2H2O The mixture of VO(acac)2 (2.65 g) and H3NTA (1.91 g) in water (40 mL) was refluxed for ca. 0.5 h. The hot solution was filtered and cooled. To this solution, an methanolic solution of 1,10-phenanthroline monohydrate (1.98 g) was added. Then, the mixture was concentrated (in order to eliminate Hacac by evaporation) and left for a crystallization at the room temperature. After 5-7 days a blue precipitate of the complex fell out. The recrystallization from hot water gave blue crystals after 4 days. The crystals of (phenH)[VO(NTA)(H2O)]∙1/2H2O were air-dried at the room temperature. The composition of the compound studied was established on the basis of the elemental analysis of carbon, hydrogen and nitrogen (Vario EL analyzer Cube CHNS). Anal. Calcd for (phenH)[VO(NTA)(H2O)]∙1/2H2O: C, 46.6%, H, 3.7%, N, 9.1%, Found: C, 46.1%, H, 3.9%, N, 9.0%.
Reference： [1]Tesmar; Inkielewicz-Stȩpniak; Sikorski; Wyrzykowski; Jacewicz; Ziȩba; Pranczk; Ossowski; Chmurzyński [Journal of Inorganic Biochemistry, 2015, vol. 152, p. 53 - 61]
  • 72
  • [ 89-73-6 ]
  • [ 3153-26-2 ]
  • [ 19161-63-8 ]
  • [ 7732-18-5 ]
  • C21H15ClN3O7V*3H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% With air; In methanol; for 2h;Reflux; [VO(acac)2] (0.01 mmol, 2.65 g) dissolved in methanol(30 mL) was added dropwise to a stirred methanolic solution(30 mL) of H2L (0.01 mol, 2.90 g). The mixture was gentlyrefluxed for 2 h, then most of the solvent was evaporated bydistillation. After cooling, the resulting brown solid wasfiltered off, washed with cold methanol, and dried in a vacuumcontaining anhydrous CaCl2. Yield: 3.35 g (62%). Anal.Calcd. for C42H42Cl2N6O17V2 (%): C, 46.90; H, 3.94; N,7.81. Found: C, 46.73; H, 3.82; N, 7.93. IR data (cm1,KBr): 3451 (br, m), 3213 (w), 1605 (vs), 1543 (w), 1493 (m),1382 (m), 1265 (m), 1146 (w), 1115 (w), 966 (m), 917 (w), 818(w), 732 (w), 656 (w), 588 (m), 576 (m), 483 (w), 464 (w), 445(w). Brown block-like single crystals of the complex, suitablefor single-crystal X-ray diffraction, were obtained by slowevaporation of a methanol solution containing the complex.
Reference： [1]Synthesis and Reactivity in Inorganic, Metal-Organic and Nano-Metal Chemistry,2016,vol. 46,p. 118 - 122
  • 73
  • [ 3153-26-2 ]
  • [ 90-02-8 ]
  • [ 75-31-0 ]
  • bis(N-isopropylsalicylaldiminato)oxovanadium(IV) [ No CAS ]
YieldReaction ConditionsOperation in experiment
89% Stage #1: salicylaldehyde; isopropylamine In methanol at 20℃; for 2h; Stage #2: bis(acetylacetonate)oxovanadium With triethylamine In methanol at 20℃; for 2h; Preparation of VOL2 A MeOH solution (20 ml) of isopropylamine (10 mmol) wasadded dropwise to a MeOH solution (20 ml) of the salicylaldehyde(10 mmol). The yellow, air stable solution was stirred for 2 h inambient temperature. Then a solution of triethylamine (15 mmol)in absolute MeOH (5 ml) was added to the solution. The mixturestirred for 10 min, and then a solution of VO(acac)2 (5 mmol) inabsolute MeOH (20 ml) was added dropwise. Upon addition, immediateprecipitation of VOL2 complex occurs. The resulting solutionwas stirred for 2 h at ambient temperature. The green powderwas isolated from the solution and purified by washing with coldmethanol. Appropriate single crystals for X-ray crystallographywere obtained directly from the reaction mixture. The typical yieldwas 89%. Anal. calc. for C20H24N2O3V: C: 61.38, H: 6.18, N: 7.16Found: C: 61.31, H: 6.21, N: 7.19.
Reference： [1]Menati, Saeid; Rudbari, Hadi Amiri; Khorshidifard, Mahsa; Jalilian, Fariba [Journal of Molecular Structure, 2016, vol. 1103, p. 94 - 102]
  • 74
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • [ 3232-36-8 ]
  • C23H16N3O5V [ No CAS ]
YieldReaction ConditionsOperation in experiment
76% Stage #1: bis(acetylacetonate)oxovanadium; salicylidene salicylhydrazide In acetonitrile for 1h; Reflux; Stage #2: 8-quinolinol In acetonitrile for 1h; Reflux; Oxidovanadium(V) complex [VO(hq)L] (3) To a 30 mL acetonitrile suspension of H2L (0.256 g, 1.00 mmol), 0.265 g (1.00 mmol) of[VO(acac)2] was added and the reaction mixture was refluxed for1 h in an oil bath, in open air. To this mixture 0.145 g (1.00 mmol) of 8-hydroxyquinoline (Hhq) was added and the reflux was continued for another hour. The resultant dark violet solution was filtered and the filtrate was kept in air. After ca. 2 d, X-ray quality dark violet single crystals were isolated, washed 3 times with cold acetonitrile and dried in open air. Yield 76% (0.353 g, based on vanadium). Anal. Calcd for C23H16N3O5V: C, 59.37; H, 3.47; N, 9.03. Found: 59.28; H,3.39; N, 8.91. Spectroscopic and ESI-MS data are given in Table 1.
Reference： [1]Sutradhar, Manas; Martins, Luísa M.D.R.S.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J.L. [Applied Catalysis A: General, 2015, vol. 493, p. 50 - 57]
  • 75
  • [ 3153-26-2 ]
  • [ 4940-11-8 ]
  • N′-(2-hydroxy-4-methoxybenzylidene)-4-hydroxybenzohydrazide [ No CAS ]
  • C23H21N2O8V [ No CAS ]
YieldReaction ConditionsOperation in experiment
53% In methanol; at 20℃; for 0.5h; General procedure: Complexes 1, 2 and 3 were prepared by the same method as described here. A methanolic solution (30mL) of VO(acac)2 (0.27g, 1.0mmol) was added to a methanolic solution (20mL) of the aroylhydrazones (1.0mmol each) and <strong>[4940-11-8]ethylmaltol</strong> (0.13g, 1.0mmol), with stirring. The mixtures were stirred at room temperature for 30min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three quarters of the solvent was evaporated. Brown block-shaped single crystals of the complexes, suitable for X-ray single crystal diffraction were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol and dried in air. Yields: 53% (1), 62% (2) and 45% (3). 1: Anal. Calc. for C23H21N2O8V: C, 54.8; H, 4.2; N, 5.6. Found: C, 54.6; H, 4.3; N, 5.5%. IR data (cm-1): 1603 (vs), 1539 (m), 1503 (m), 1455 (w), 1407 (m), 1343 (m), 1256 (s), 1176 (m), 1116 (m), 1029 (m), 976 (s), 836 (m), 754 (w), 732 (w), 715 (w), 645 (m), 469 (m). UV (lambda, epsilon): 215nm, 2.94×104L·mol-1·cm-1; 286nm, 2.71×104L·mol-1·cm-1; 348nm, 1.31×104L·mol-1·cm-1; 460nm, 7.18×103L·mol-1·cm-1. 1H NMR (300MHz, d6-DMSO): delta 9.01 (s, 1H, maltol-CH), 8.45 (d, 1H, CH=N), 7.78-7.69 (m, 3H, ArH), 7.00 (d, 2H, ArH), 6.68-6.64 (m, 2H, ArH), 6.48 (d, 1H, maltol-CH), 3.81 (d, 6H, OCH3), 3.00 (q, 2H, CH2CH3), 1.33 (t, 3H, CH2CH3).
Reference： [1]Polyhedron,2015,vol. 97,p. 268 - 272
  • 76
  • [ 3153-26-2 ]
  • [ 4940-11-8 ]
  • N′-(3-ethoxy-2-hydroxybenzylidene)pivalohydrazide [ No CAS ]
  • C21H25N2O7V [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% In methanol; at 20℃; for 0.5h; General procedure: Complexes 1, 2 and 3 were prepared by the same method as described here. A methanolic solution (30mL) of VO(acac)2 (0.27g, 1.0mmol) was added to a methanolic solution (20mL) of the aroylhydrazones (1.0mmol each) and <strong>[4940-11-8]ethylmaltol</strong> (0.13g, 1.0mmol), with stirring. The mixtures were stirred at room temperature for 30min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three quarters of the solvent was evaporated. Brown block-shaped single crystals of the complexes, suitable for X-ray single crystal diffraction were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol and dried in air. Yields: 53% (1), 62% (2) and 45% (3).
Reference： [1]Polyhedron,2015,vol. 97,p. 268 - 272
  • 77
  • [ 3153-26-2 ]
  • [ 4940-11-8 ]
  • 2-bromo-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • C23H20BrN2O7V [ No CAS ]
YieldReaction ConditionsOperation in experiment
45% In methanol; at 20℃; for 0.5h; General procedure: Complexes 1, 2 and 3 were prepared by the same method as described here. A methanolic solution (30mL) of VO(acac)2 (0.27g, 1.0mmol) was added to a methanolic solution (20mL) of the aroylhydrazones (1.0mmol each) and <strong>[4940-11-8]ethylmaltol</strong> (0.13g, 1.0mmol), with stirring. The mixtures were stirred at room temperature for 30min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three quarters of the solvent was evaporated. Brown block-shaped single crystals of the complexes, suitable for X-ray single crystal diffraction were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol and dried in air. Yields: 53% (1), 62% (2) and 45% (3).
Reference： [1]Polyhedron,2015,vol. 97,p. 268 - 272
  • 78
  • [ 89-73-6 ]
  • [ 3153-26-2 ]
  • N′-(3-bromo-2-hydroxybenzylidene)isonicotinohydrazide [ No CAS ]
  • C20H14BrN4O6V*2H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
55% In methanol; water; for 0.5h;Reflux; A hot methanol solution (15 mL) of VO(acac)2 (1 mM, 0.26 g) was added to a hot methanolsolution (15 mL) of H2L (1 mM, 0.32 g). Then, 2-hydroxybenzohydroxamic acid(1 mM, 0.15 g) dissolved in 10 mL of water was added to the solution. The mixture wasstirred for 30 min at reflux, and then cooled to room temperature, to give a brown solution.Single crystals of the complex, suitable for X-ray diffraction, were formed by slow evaporationof the methanol solution containing the complex in air for few days. Yield: 55%. Anal.Calcd for C20H18BrN4O8 V: C, 41.9; H, 3.2; N, 9.8. Found: C, 41.7; H, 3.1; N, 9.9%.
Reference： [1]Journal of Coordination Chemistry,2014,vol. 67,p. 3279 - 3287
  • 79
  • [ 3153-26-2 ]
  • [ 495-18-1 ]
  • [ 1829-34-1 ]
  • [ 5814-05-1 ]
  • [VO(N'-(3-bromo-2-hydroxybenzylidene)-2-chlorobenzohydrazide(-2H))(benzohydroxamic acid(-H))] [ No CAS ]
YieldReaction ConditionsOperation in experiment
53% In methanol at 20℃; Darkness; Synthesis of I 3-Bromosalicylaldehyde (1.0 mmol, 201 mg), 2-chlorobenzohydrazide (1.0 mmol, 171 mg) and benzohydroxamic acid (1.0 mmol, 137 mg) were dissolved in methanol (20 mL) and stirred at room temperature for 10 min. Then, 20 mL methanolic solution containing [VO(Acac)2] (1.0 mmol, 265 mg) was added dropwise to the solution. The mixture was further stirred at room temperature for 10 min to give a deep brown solution. The solution was filtered to obtain clear filtrate, which was kept still at dark to slow evaporation. A few days later, well-shaped brown single crystals of the complex were formed and separated by filtration. The product was washed three times with cold methanol and dried in air. The yield was 53%. UV-Vis (acetonitrile; λmax (logε)): 240 (5.19); 269 (4.14); 341 (3.75); 455 (3.64) nm. IR (KBr; ν, cm-1) 3534 m, 3135 w, 1609 v.s, 1554 m, 1517 w, 1468 m, 1401 s, 1346 s, 1266 m, 1235 w, 1162 w, 1118 m, 1039 w, 965 m, 910 w, 825 m, 776 w, 739 w, 696 m, 579 s, 450 w. For C21H14N3O5ClBrV (I) anal. calcd., %: C, 45.47; H, 2.54; N, 7.58. Found, %: C, 45.32; H, 2.63; N, 7.50.
Reference： [1]Qian; Ye; Huo; You; Zhu [Russian Journal of Coordination Chemistry/Koordinatsionnaya Khimiya, 2015, vol. 41, # 1, p. 58 - 63][Koord. Khim.]
  • 80
  • [ 3153-26-2 ]
  • [ 5970-45-6 ]
  • zinc vanadate [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: bis(acetylacetonate)oxovanadium; zinc(II) acetate dihydrate With polyvinylpyrrolidone In ethanol; N,N-dimethyl-formamide at 20℃; for 8h; Stage #2: at 500℃; for 4h; Polyvinylpyrrolidone was dissolved in DMF and ethanol mixtures by magnetic stirring for 5 h to form a 15 wt% solution. Subsequently, stoichiometric amounts of reagents were added to the PVP solution, followed by vigorously stirring at room temperature for 8 h until the complete dissolution of the solid reagents to obtain a uniform solution.Then, the above solution was loaded into a 20 mL syringe and electrospunned. The electrospinning was performed in open environment at room temperature. Finally, the obtained composite nanofibers were annealed in air atmosphere for 4 h at 500°C to produce Zn2V2O7 nanofibers.
Reference： [1]Luo, Lei; Fei, Yaqian; Chen, Ke; Li, Dawei; Wang, Xin; Wang, Qingqing; Wei, Qufu; Qiao, Hui [Journal of Alloys and Compounds, 2015, vol. 649, p. 1019 - 1024]
  • 81
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • N'-(3-bromo-5-chloro-2-hydroxybenzylidene)nicotinohydrazide [ No CAS ]
  • C22H13BrClN4O4V [ No CAS ]
YieldReaction ConditionsOperation in experiment
70% In methanol at 20℃; for 0.5h; Synthesis of [VOL1L'] (1) General procedure: A methanolic solution (10 mL) of [VO(acac)2] (0.1 mmol,26.5 mg) was added to a methanolic solution (10 mL) ofH2L1(0.1 mmol, 25.9 mg) and HL’ (0.1 mmol, 14.5 mg)with stirring. The mixture was stirred for 30 min at roomtemperature to give a deep brown solution. The resultingsolution was allowed to stand in air for a few days. Brownblock-shaped crystals suitable for X-ray single crystal diffraction were formed at the bottom of the vessel. The isolatedproducts were washed three times with cold ethanol, anddried in air. Yield: 55%
Reference： [1]Sheng, Gui-Hua; Han, Xiao; Ye, Yu-Ting; Ren, Jin-Qi; You, Zhong-Lu; Zhu, Hai-Liang [Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 2016, vol. 46, # 8, p. 1129 - 1132]
  • 82
  • [ 3153-26-2 ]
  • C10H13NOS [ No CAS ]
  • C20H22N2O4S2V2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
69% In ethanol at 57℃; for 6h; Inert atmosphere; Synthesis of the nickel complex, B General procedure: A methanolic solution (5 mL) of Ni(OAc)2*4H2O (0.076 g, 0.307 mmol) was added dropwise to a solution (5 mL) of the Schiff base A (0.062 g, 0.307 mmol). The resulting brown solution was stirred for 5 h while heating at 55 °C and then left to stand overnight. The oily brown precipitate was washed with methanol and finally dried in vacuo (yield: 68 %)
Reference： [1]Mohammadtabar, Fatemeh; Shafaatian, Bita; Soleymanpour, Ahmad; Rezvani, S. Ahmad; Notash, Behrouz [Transition Metal Chemistry, 2016, vol. 41, # 4, p. 475 - 484]
  • 83
  • [ 3153-26-2 ]
  • [ 201530-41-8 ]
  • [V(V)O(μ-4-[3,5-bis(2-hydroxyphenyl)-1,2,4-triazol-1-yl]benzoic acid)(OMe)]2 [ No CAS ]
Reference： [1]European Journal of Inorganic Chemistry,2016,vol. 2016,p. 1430 - 1441
  • 84
  • [ 3153-26-2 ]
  • [ 546-88-3 ]
  • 2-chloro-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • C18H17ClN3O6V [ No CAS ]
YieldReaction ConditionsOperation in experiment
56% Stage #1: bis(acetylacetonate)oxovanadium; acetylhydroxamic acid; 2-chloro-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide In methanol at 20℃; for 0.5h; Stage #2: With air In methanol 2.2. Synthesis of the complexes General procedure: Complexes 1, 2, and 3 were prepared by the method described here. A methanolic solution (30 mL) of VO(acac)2 (0.27 g, 1.0 mmol) was added to a methanolic solution (20 mL) of H2L (0.32 g, 1.0 mmol) and the bidentate ligands (1.0 mmol each), with stirring. The mixtures were stirred at room temperature for30 min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three-quarters of the solvent evaporated. Brown block-shaped single crystals of the complexes,suitable for X-ray single-crystal diffraction, were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol, and dried in air. Yields: 2.56 g, 56% (1);3.71 g, 73% (2); 3.56 g, 68% (3).
Reference： [1]You, Zhonglu; Zheng, Boyang; Yang, Ting; Liu, Fang; Cheng, Xiao-Shan [Journal of Coordination Chemistry, 2016, vol. 69, # 8, p. 1371 - 1379]
  • 85
  • [ 118-71-8 ]
  • [ 3153-26-2 ]
  • 2-chloro-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • C22H18ClN2O7V [ No CAS ]
YieldReaction ConditionsOperation in experiment
73% Stage #1: Maltol; bis(acetylacetonate)oxovanadium; 2-chloro-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide In methanol at 20℃; for 0.5h; Stage #2: With air In methanol 2.2. Synthesis of the complexes General procedure: Complexes 1, 2, and 3 were prepared by the method described here. A methanolic solution (30 mL) of VO(acac)2 (0.27 g, 1.0 mmol) was added to a methanolic solution (20 mL) of H2L (0.32 g, 1.0 mmol) and the bidentate ligands (1.0 mmol each), with stirring. The mixtures were stirred at room temperature for30 min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three-quarters of the solvent evaporated. Brown block-shaped single crystals of the complexes,suitable for X-ray single-crystal diffraction, were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol, and dried in air. Yields: 2.56 g, 56% (1);3.71 g, 73% (2); 3.56 g, 68% (3).
Reference： [1]You, Zhonglu; Zheng, Boyang; Yang, Ting; Liu, Fang; Cheng, Xiao-Shan [Journal of Coordination Chemistry, 2016, vol. 69, # 8, p. 1371 - 1379]
  • 86
  • [ 3153-26-2 ]
  • [ 4940-11-8 ]
  • 2-chloro-N′-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • C23H20ClN2O7V [ No CAS ]
YieldReaction ConditionsOperation in experiment
68% General procedure: Complexes 1, 2, and 3 were prepared by the method described here. A methanolic solution (30 mL) of VO(acac)2 (0.27 g, 1.0 mmol) was added to a methanolic solution (20 mL) of H2L (0.32 g, 1.0 mmol) and the bidentate ligands (1.0 mmol each), with stirring. The mixtures were stirred at room temperature for30 min to give deep brown solution. The resulting solution was allowed to stand in air for a few days until three-quarters of the solvent evaporated. Brown block-shaped single crystals of the complexes,suitable for X-ray single-crystal diffraction, were formed at the bottom of the vessel. The crystals were isolated by filtration, washed three times with cold methanol, and dried in air. Yields: 2.56 g, 56% (1);3.71 g, 73% (2); 3.56 g, 68% (3).
Reference： [1]Journal of Coordination Chemistry,2016,vol. 69,p. 1371 - 1379
  • 87
  • [ 3153-26-2 ]
  • [ 495-18-1 ]
  • 2-bromo-N′-(2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • [VO(2-bromo-N'-(2-hydroxybenzylidene)benzohydrazide)benzohydroxamate] [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% In methanol at 20℃; for 0.5h; Synthesis of Complex 1 To a methanolic solution (10 mL) of L (0.1 mmol, 31.8 mg)and benzohydroxamic acid (0.1 mmol, 13.7 mg) was added amethanolic solution (10 mL) of VO(acac)2 (0.1 mmol,26.5 mg) with continuous stirring. The mixture was stirredfor 30 min at room temperature to give a deep brown solution. Upon keeping the solution in air for about a week,brown block-like single crystals suitable for X-ray diffractionwere deposited at the bottom of the vessel. The isolated product was washed three times with cold methanol, and dried ina vacuum over anhydrous CaCl2. Anal. Calcd. forC21H15BrN3O5V (FW 520.2): C, 48.5; H, 2.9; N, 8.1. Found:C, 48.3; H, 3.0; N, 8.0%. Yield, 31.3 mg (60% on the basis ofV). IR data (cm1, KBr): 3124, 1602, 1536, 1473, 1393, 1347,1280, 1140, 1117, 1028, 977, 908, 759, 690, 593, 481. UV-Vis(acetonitrile, c D5.2 £105mol¢L1): λmax(e) D270(10730), 332 (4670), 445 (3462) nm (mol1Lcm1).
Reference： [1]Sun, Yu-Bing; Xie, Qing; Li, Wei; Ding, Yi; Ye, Yu-Ting [Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 2016, vol. 46, # 11, p. 1613 - 1617]
  • 88
  • [ 148-24-3 ]
  • [ 3153-26-2 ]
  • 2-bromo-N′-(2-hydroxybenzylidene)benzohydrazide [ No CAS ]
  • [VO(2-bromo-N'-(2-hydroxybenzylidene)benzohydrazide)8-hydroxyquinoline] [ No CAS ]
YieldReaction ConditionsOperation in experiment
69% In methanol at 20℃; for 0.5h; Synthesis of Complex 2 To a methanolic solution (10 mL) of L (0.1 mmol, 31.8 mg)and 8-hydroxyquinoline (0.1 mmol, 14.5 mg) was added amethanolic solution (10 mL) of VO(acac)2(0.1 mmol,26.5 mg), with continuous stirring. The mixture was stirredfor 30 min at room temperature to give a deep brown solution. Upon keeping the solution in air for about a week,brown block-like single crystals suitable for X-ray diffractionwere deposited at the bottom of the vessel. The isolated product was washed three times with cold methanol, and dried ina vacuum over anhydrous CaCl2. Anal. Calcd. forC23H15BrN3O4V (FW 528.2): C, 52.3; H, 2.9; N, 8.0. Found:C, 52.2; H, 2.8; N, 8.1%. Yield, 36.7 mg (69% on the basis ofV). IR data (cm1, KBr): 1598, 1549, 1504, 1462, 1429, 1378,1339, 1275, 1210, 1149, 1098, 1026, 962, 898, 816, 774, 643,585. UV-Vis (acetonitrile, c D3.3 £105mol¢L1):λmax(e) D242 (53345), 275 (27115), 330 (13800), 550 (7208)nm (mol1Lcm1).
Reference： [1]Sun, Yu-Bing; Xie, Qing; Li, Wei; Ding, Yi; Ye, Yu-Ting [Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 2016, vol. 46, # 11, p. 1613 - 1617]

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