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CAS No. : | 2170398-07-7 | MDL No. : | MFCD34179497 |
Formula : | C14H10N2O8 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SMGIBNSQLDHHHU-UHFFFAOYSA-N |
M.W : | 334.24 | Pubchem ID : | 139174717 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P264-P270-P280-P301+P312+P330-P305+P351+P338-P337+P313-P501 | UN#: | N/A |
Hazard Statements: | H302-H319 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | at 150℃; for 72h; Autoclave; | 2.3.1 Synthesis of [Co2(dpb)(dipe)(H2O)2]n (1) A mixture of Co(NO3)2·6H2O (145.5mg, 0.5mmol), H4dpb (66.84mg, 0.2mmol), dipe (36.4mg, 0.2mmol) and H2O (8mL) was sealed in a 25mL Teflon-lined stainless steel reactor and heated to 150°C for 72h. Purple sheet crystals of 1 were obtained in 60% yield (based on H4dpb) when the mixture cooled to room temperature, washed with deionized water several times and dried in air. Anal. Calc. for Co2C26H20N4O10 (666.32): C, 46.83; H, 3.06; N, 8.38. Found: C, 46.87; H, 3.03; N, 8.41%. IR (KBr, cm-1): 3435(m), 1602(s), 1552(w), 1492(w), 1357(s), 1120(w), 1019(w), 972(w), 838(s), 783(w), 737(s). The IR spectra of complex 1 is presented in the Supporting Information (Fig. S2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42% | at 150℃; for 72h; Autoclave; | 2.3.1 Synthesis of [Co2(dpb)(dipe)(H2O)2]n (1) General procedure: A mixture of Co(NO3)2·6H2O (145.5mg, 0.5mmol), H4dpb (66.84mg, 0.2mmol), dipe (36.4mg, 0.2mmol) and H2O (8mL) was sealed in a 25mL Teflon-lined stainless steel reactor and heated to 150°C for 72h. Purple sheet crystals of 1 were obtained in 60% yield (based on H4dpb) when the mixture cooled to room temperature, washed with deionized water several times and dried in air. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | In N,N-dimethyl-formamide at 110℃; for 72h; Autoclave; | 2.3.2 Synthesis of [Zn2(dpb)(dipe)(H2O)2]n (2) A mixture of Zn(NO3)2·6H2O (148.7mg, 0.5mmol), H4dpb (66.84mg, 0.2mmol), dipe (36.4mg, 0.2mmol), H2O (7mL) and DMF (1mL) was sealed in a 25mL Teflon-lined stainless steel reactor and heated to 110°C for 72h. Colorless block-shaped crystals of 2 were obtained in 51% yield (based on H4dpb) when the mixture cooled to room temperature, washed with deionized water, and dried in air. Anal. Calc. for Zn2C26H20N4O10 (679.20): C, 45.95; H, 3.02; N, 8.29. Found: C, 45.98; H, 2.97; N, 8.25%. IR (KBr, cm-1): 3431(m), 1603(s), 1491(w), 1431(w), 1356(s), 1118(w), 1067(w), 1029(m), 969(m), 835(m), 738(m). The IR spectra of complex 1 is existed in the Supporting Information (Fig. S3). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | The ligand of 1-(3,5-dicarboxybenzyl)-1H-pyrazole-3,5-dicarboxylic acid(H4dpb) was synthesized according to the following procedure [26]. Potassium hydroxide (KOH) (0.28g, 5mmol) was added to a solution of <strong>[4077-76-3]dimethyl 1H-pyrazole-3,5-dicarboxylate</strong> (0.46g, 2.5mmol) in 20mL DMF. The mixture was then stirred for 30min at 80C, following which dimethyl 5-(bromomethyl)isophthalate (0.71g, 2.5mmol) was added and the solution was stirred further for 2h at 80C, then 5mL water and KOH (1.12g, 20mmol) were added into the resulting mixture, the reaction mixture was refluxed for 3h. The solution was cooled down to room temperature and then poured into water of 2C approximately (300mL), acidified with HCl (6.0mol/L) to pH 5-6, the numerous white solid of H4dpb was collected by filtration and washed by water with a yield of 0.71g (85.0%). ESI-MS: m/z (100%) 333.06 [M-1]+. The IR spectra of H4dpb is given in the Supporting Information (Fig. S1). IR (KBr, cm-1): 3487(m), 3151(s), 1707(s), 1533(w), 1471(w), 1458(m), 1383(w), 1228(s), 1107(m), 1006(w), 912(w), 804(s), 770(s). 742(m) (see Scheme1 ). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76% | In water; acetonitrile at 95℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | In water; acetonitrile at 95℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In water; acetonitrile at 95℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
69% | at 120℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid In ethanol; water at 160℃; for 72h; High pressure; Autoclave; | Synthesis of ZJU-158 General procedure: As Rare Earth element, both of Terbium and Europium possess great luminescent properties. And also it's easy to observe their strong green or red luminescence by naked eyes. Thus we chose to synthesize and research Eu- and Tb-based MOFs respectively, and emphasized ZJU-158-Tb because of its better detection sensitivity to UA. ZJU-158-Tb was prepared by a solvothermal technique. Typically, a mixture of Tb(NO3)3·6H2O (45 mg, 0.1 mmol), ligand L (16.7 mg, 0.05 mmol),N,N-dimethylformamide (DMF) (30 mL), ethyl alcohol (EtOH) (10mL), deionized water (H2O) (15 mL) and acetic acid (CH3COOH) (1mL) was sealed into an 80 mL glass bottle and ultrasonically dissolved to form clarified solution. Then the solution was loaded into 25 mLTeflon-lined stainless-steel autoclaves and heated at a 160 °C oven for 72 h. After the solvothermal growth and overnight cooling in air to room temperature, the colourless bulk crystals were collected by filtration and washing with DMF and EtOH for several times. TheZJU-158-Eu was obtained through the same procedure with ZJU-158-Tb except replacing the metal salt Tb(NO3)3·6H2O to Eu(NO3)3·6H2O and it had the same morphology. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid In ethanol; water at 160℃; for 72h; High pressure; Autoclave; | Synthesis of ZJU-158 General procedure: As Rare Earth element, both of Terbium and Europium possess great luminescent properties. And also it's easy to observe their strong green or red luminescence by naked eyes. Thus we chose to synthesize and research Eu- and Tb-based MOFs respectively, and emphasized ZJU-158-Tb because of its better detection sensitivity to UA. ZJU-158-Tb was prepared by a solvothermal technique. Typically, a mixture of Tb(NO3)3·6H2O (45 mg, 0.1 mmol), ligand L (16.7 mg, 0.05 mmol),N,N-dimethylformamide (DMF) (30 mL), ethyl alcohol (EtOH) (10mL), deionized water (H2O) (15 mL) and acetic acid (CH3COOH) (1mL) was sealed into an 80 mL glass bottle and ultrasonically dissolved to form clarified solution. Then the solution was loaded into 25 mLTeflon-lined stainless-steel autoclaves and heated at a 160 °C oven for 72 h. After the solvothermal growth and overnight cooling in air to room temperature, the colourless bulk crystals were collected by filtration and washing with DMF and EtOH for several times. The ZJU-158-Eu was obtained through the same procedure with ZJU-158-Tb except replacing the metal salt Tb(NO3)3·6H2O to Eu(NO3)3·6H2O and it had the same morphology. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
71% | In acetonitrile at 120℃; for 72h; High pressure; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | With water; barium(II) acetate In acetonitrile at 95℃; for 72h; High pressure; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With water; barium(II) acetate In acetonitrile at 95℃; for 72h; High pressure; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | In acetonitrile at 95℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | In acetonitrile at 120℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | at 160℃; for 72h; Sealed tube; Autoclave; High pressure; | 3.3. Synthesis of [Me2NH2][LnL]2H2O}n (Ln = Eu 1, Tb 2, Dy 3, Gd 4) (Compounds 1-4) General procedure: In total, 45 mg of Ln(NO3)36H2O and 33 mg of H4L were dissolved in DMF (N,Ndimethylformamide)(5 mL) and H2O (5 mL). The solution was sealed in a 25-mL Teflonlinedstainless-steel autoclave, and heated at 160 C for 72 h. Then the mixture wascooled to room temperature at a rate of 1 C/min. The resulting colorless crystals,[Me2NH2][LnL]2H2O}n, were washed with DMF and methanol several times, and thenevacuated to remove the co-assembled DMF and methanol in the pores of MOFs. Theyields are 68%, 72%, 76%, and 75% for compounds 1-4 based on the metal ions. Elementalanalysis (%) calculated for the various crystals are listed as follows. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | at 160℃; for 72h; Sealed tube; Autoclave; High pressure; | 3.3. Synthesis of [Me2NH2][LnL]2H2O}n (Ln = Eu 1, Tb 2, Dy 3, Gd 4) (Compounds 1-4) General procedure: In total, 45 mg of Ln(NO3)36H2O and 33 mg of H4L were dissolved in DMF (N,Ndimethylformamide)(5 mL) and H2O (5 mL). The solution was sealed in a 25-mL Teflonlinedstainless-steel autoclave, and heated at 160 C for 72 h. Then the mixture wascooled to room temperature at a rate of 1 C/min. The resulting colorless crystals,[Me2NH2][LnL]2H2O}n, were washed with DMF and methanol several times, and thenevacuated to remove the co-assembled DMF and methanol in the pores of MOFs. Theyields are 68%, 72%, 76%, and 75% for compounds 1-4 based on the metal ions. Elementalanalysis (%) calculated for the various crystals are listed as follows. [Me2NH2][EuL]2H2O}n (1) Elemental analysis (%): calcd for C16H18EuN3O10, C,34.06; H, 3.22; N, 7.45. Found: C, 34.31; H, 3.12; N, 7.50. Infrared (KBr pellet, cm1):3626(w), 3390(m), 3153(w), 3064(m), 2999(m), 2796(m), 2476(w), 1909(w), 1570(s), 1460(s),1301(s), 850(s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | at 160℃; for 72h; Sealed tube; Autoclave; High pressure; | 3.3. Synthesis of [Me2NH2][LnL]2H2O}n (Ln = Eu 1, Tb 2, Dy 3, Gd 4) (Compounds 1-4) General procedure: In total, 45 mg of Ln(NO3)36H2O and 33 mg of H4L were dissolved in DMF (N,Ndimethylformamide)(5 mL) and H2O (5 mL). The solution was sealed in a 25-mL Teflonlinedstainless-steel autoclave, and heated at 160 C for 72 h. Then the mixture wascooled to room temperature at a rate of 1 C/min. The resulting colorless crystals,[Me2NH2][LnL]2H2O}n, were washed with DMF and methanol several times, and thenevacuated to remove the co-assembled DMF and methanol in the pores of MOFs. Theyields are 68%, 72%, 76%, and 75% for compounds 1-4 based on the metal ions. Elementalanalysis (%) calculated for the various crystals are listed as follows. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76% | at 160℃; for 72h; Sealed tube; Autoclave; High pressure; | 3.3. Synthesis of [Me2NH2][LnL]2H2O}n (Ln = Eu 1, Tb 2, Dy 3, Gd 4) (Compounds 1-4) General procedure: In total, 45 mg of Ln(NO3)36H2O and 33 mg of H4L were dissolved in DMF (N,Ndimethylformamide)(5 mL) and H2O (5 mL). The solution was sealed in a 25-mL Teflonlinedstainless-steel autoclave, and heated at 160 C for 72 h. Then the mixture wascooled to room temperature at a rate of 1 C/min. The resulting colorless crystals,[Me2NH2][LnL]2H2O}n, were washed with DMF and methanol several times, and thenevacuated to remove the co-assembled DMF and methanol in the pores of MOFs. Theyields are 68%, 72%, 76%, and 75% for compounds 1-4 based on the metal ions. Elementalanalysis (%) calculated for the various crystals are listed as follows. |