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Structure of 10049-08-8 * Storage: {[proInfo.prStorage]}
* 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.
Reference:
[1] Collection of Czechoslovak Chemical Communications, [2] Collection of Czechoslovak Chemical Communications, 1960, vol. 25, p. 2155 - 2160
[3] , Gmelin Handbook: Na: SVol.3, 1.2.5, page 912 - 916,
19
[ 10049-08-8 ]
[ 1165952-91-9 ]
[ 37366-09-9 ]
Reference:
[1] Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1987, vol. 36, p. 1922 - 1926[2] Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1987, p. 2071 - 2076
[3] Russian Chemical Bulletin, 2005, vol. 54, # 10, p. 2374 - 2378
(3S)-3-(1,3-benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic Acid[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With potassium hydroxide; dipotassium peroxodisulfate; potassium hexacyanoferrate(III) In tetrahydrofuran; aqueous KOH; water; acetone; toluene; butan-1-ol
13 Synthesis of (3S)-3-(1,3-benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic Acid
Example 13 Synthesis of (3S)-3-(1,3-benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic Acid Step One: To a solution of 3-benzylpyridine (1.65 g, 9.77 mmol) in acetone (3.5 mL), 1-chloro-2,4-dinitrobenzene (2.00 g, 9.56 mmol) was added and the mixture was refluxed overnight. The mixture was cooled to room temperature, diluted with acetone and the solvent was decanted from the precipitate. The crude solid was washed with acetone (2 times) and diethyl ether (1 time), decanting each time to give 37(3.57 g, 100%) as a gray solid. Step Two: To a solution of 1-amino-1-hydroxymethylcyclohexane (0.45 g, 3.5 mmol) in n-butanol (8.75 mL), solid N-(2,4-dintrophenyl)-3-benzylpyridinum chloride (37, 1.23 g, 3.3 mmol) was added. The resulting solution was heated to reflux for 2.5 days under a nitrogen atmosphere. The mixture was cooled, diluted with water and filtered. The filtrate was basified with concentrated NH4OH (2 mL) and extracted with ethyl acetate. The aqueous layer was concentrated to dryness to give 38(0.56 g) as a yellow oil which was used without further purification. Step Three: To a solution of crude 38(0.56 g, 3.5 mmol theoretical) in water (10 mL), a solution of potassium ferricyanide (3.3 g, 10 mmol) in water (15 mL) was added dropwise via an addition funnel over 30 minutes at 0° C. A solution of KOH (0.76 g, 13.5 mmol) in water (5 mL) was then added over 30 minutes. Toluene (10 mL) was added and the solution was stirred for one hour at 0° C. The layers were separated, and the aqueous layer was extracted again with toluene. The combined extracts were dried over Na2SO4 and filtered and the filtrate was concentrated under reduced pressure. The residue was chromatographed on silica gel, eluding with 7:13 hexanes:ethyl acetate to give 39(20 mg, 1.9%, two steps.) Step Four: To a suspension of 39(20 mg, 0.068 mmol) in aqueous KOH (1M, 0.70 mL) potassium persulfate (0.073 g, 0.270 mmol) and ruthenium (III) chloride (1 mg, catalytic) and THF (0.25 mL) were added. The mixture was stirred for 1 hour and extracted with dichloromethane. The aqueous layer was acidified and extracted with ethyl acetate (3 times). The ethyl acetate extracts were combined, dried over MgSO4 and filtered. The filtrate was concentrated under reduced pressure to give 40(0.0148 g, 70%) as a tan solid. (3S)-3-(1,3-Benzodioxol-5-yl)-3-[({1-[2-oxo-3-(phenylmethyl)-1(2H)-pyridinyl]cyclohexyl}carbonyl)amino]propanoic acid was prepared from 40according to the procedures described in Example 1. 1H NMR (400 MHz, CD3SO2CD3): δ 1.40 (m, 4H), 1.68 (m, 2H), 2.04 (m, 2H), 2.60 (d, J=7.0 Hz, 2H), 3.67 (d, J=15.2 Hz, 1H), 3.72 (d, J=15.2 Hz, 1H), 5.12 (m, 1H), 5.95 (m, 2H), 6.19 (t, J=7.0 Hz, 1H), 6.74 (dd, J=7.8, 1.4 Hz, 1H), 6.76 (d, J=7.8 Hz, 1H), 6.90 (d, J=1.4 Hz, 1H), 7.10 (d, J=5.8 Hz, 1H), 7.20 (m, 5H), 7.57 (d, J=8.4Hz, 1H), 7.66 (dd, J=7.7, 1.8 Hz, 1H).
With sodium periodate In tetrachloromethane; water; acetonitrile
44.2 1-tert-Butoxycarbonyl-4-ethoxycarbonylpiperidin-4-ylacetic Acid
Step 2 1-tert-Butoxycarbonyl-4-ethoxycarbonylpiperidin-4-ylacetic Acid To a solution of sodium periodate (14.69 g) in a mixture of water (90 ml), carbon tetrachloride (50 ml) and acetonitrile (50 ml) was added ruthenium chloride (111 mg) and a solution of 4-allyl-4-ethoxycarbonylpiperidine-1-carboxylic acid tert-butyl ester (5.07 g) in a mixture of carbon tetrachloride (10 ml) and acetonitrile (10 ml) was added dropwise, and the mixture was stirred at room temperature for 1.5 hours. After completion of the reaction, the reaction mixture was filtrated and the residue was washed with ethyl acetate. The aqueous layer of the obtained filtrate was removed and the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (ethyl acetate) and dried under reduced pressure to give the title compound (4.23 g). 1H-NMR (δ ppm, CDCl3) 1.26 (tr, J=7.0 Hz, 3H), 1.48-1.57 (m, 11H), 2.05-2.18 (m, 2H), 2.65 (s, 2H), 3.21 (m, 2H), 3.65-3.75 (m, 2H), 4.19 (q, J=7.0 Hz, 2H).
With caesium carbonate In methanol other Radiation; mixt. of RuCl3, Cs2CO3 and MeOH was sealed in microwave app.; CO (50 psi) was introduced; sealed; heated with stirring to 110°C using power of 300 W; held for 10 min; cooled to 50°C; evapd. (vac.); hexane added; heated; solvent removed;
With Cu or Zn In ethanol other Radiation; γ irradiation of 1E-3 mol/l RuCl3 in ethanol under CO atmosphere at room temp. in presence of Cu or Zn powder;
With zinc In methanol heating RuCl3 with Zn at a CO pressure of 5-10 atm at 65 °C for 30 h;; extraction of thr solid residue of the filtration; pptn. on concentrating;;
With Zn In methanol heating RuCl3 with Zn at a CO pressure of 5-10 atm at 65 °C for 30 h;; extraction of thr solid residue of the filtration; pptn. on concentrating;;
In N,N-dimethyl-formamide RuCl3 refluxed in DMF with a twofold excess of the org. compd. for 4-6 h; solvent removed, thoroughly washed with ether, dissolved in alkaline water (pH 10), isolated upon lowering of the pH to 3.5;
In N,N-dimethyl-formamide RuCl3 refluxed in DMF with a threefold excess of the org. compd. for 4-6 h; solvent removed, thoroughly washed with ether, dissolved in alkaline water (pH 10), isolated upon lowering of the pH to 3.5;
In water an excess of KI is added to an aq. soln. of RuCl3 which is stirred for 0.5 h, then warmed for 0.5 h on a water bath; solid is filtered, washed with distd. water, dried over fused CaCl2;
With methanol; [2,2]bipyridinyl In methanol react. of RuCl3 and bpy in MeOH; recrystn. from MeOH;
With [2,2]bipyridinyl In N,N-dimethyl-formamide stoichiometric ratio, reflux; evapn. to dryness, redissolved in ethanol, chromy., solvent was stripped;
In sulfuric acid boiling commercial Ru chloride (40 % RuCl3, 60 % RuCl4) with bipyridyl in diluted H2SO4 soln. (pH 2); at first formation of (Ru(bpy))(3+), then green (Ru(H2O)2(bpy)2)(3+) and on further heating (Ru(bpy)2)(2+); react. completed after 15 h;;
With sodium sulfite In sulfuric acid react. of commercial Ru chloride with bipyridyl in H2SO4; react. without formation of internmediates;;
In hydrogenchloride react. of commercial Ru chloride with bipyridyl in n-HCl soln.; direct react. without intermediate with an excess of bipyridyl;;
In hydrogenchloride react. of commercial Ru chloride with bipyridyl in n-HCl soln.; intermediate red (RuCl2(bpy)2)(1+);;
With potassium hydrogencarbonate In ethanol; water RuCl3 in EtOH and water was refluxed for 4-5 h. An excess amount of theligand was added to the blue soln. and the mixture was refluxed until its color turned red. After cooling KHCO3 was added in several portions, followed always by 1-3 h reflux.; concn., filtration, extn.(benzene),The extn. was chromd., evapn. ,recrystn. (EtOH);
In ethylene glycol; acetonitrile a soln. of RuCl3 in ethylene glycol reacted with a soln. of ligand in MeCN at 150°C for 15 h; not isolated, detected by absorption and emission spectroscopy;
With potassium hydrogencarbonate In ethanol; water RuCl3 in EtOH and water was refluxed for 4-5 h. An excess amount of theligand was added to the blue soln. and the mixture was refluxed until its color turned red. After cooling KHCO3 was added in several portions, followed always by 1-3 h reflux.; concn., filtration, extn.(benzene),The extn. was chromd., evapn. ,recrystn. (EtOH);
{(C12H12)2Ru}(2+)*2{PF6}(1-)={(C12H12)2Ru}{PF6}2[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With aluminium trichloride; aluminium In neat (no solvent) melting a mixt. of RuCl3, AlCl3, Al powder and 2.3-dimethyl naphthalene under addn. of a small amount of hexamethyl benzene as catalyst; hydrolysis; pptn. with NH4PF6;;
With Al; AlCl3 In neat (no solvent) melting a mixt. of RuCl3, AlCl3, Al powder and 2.3-dimethyl naphthalene under addn. of a small amount of hexamethyl benzene as catalyst; hydrolysis; pptn. with NH4PF6;;
[Ru(4'-(4-methylcarboxyphenyl)-2,2':6',2''-terpyridine)2][PF6]2[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
72%
With silver nitrate In N,N-dimethyl-formamide reflux for 2 h, 0.5 equiv. of RuCl3 and 3 equiv. of AgNO3, column. chromy. and anion exchange with NH4PF6;
In methanol a cooled soln. of RuCl3 in MeOH is added drop by drop to a methanolic soln. of the ligand in ice cold condition with stirring, mixt. is stirredfor 1 h; soln. is concd. at room temp., compd. is filtered, washed with water and hot benzene, dried over fused CaCl2; elem. anal.;
In ethanol other Radiation; to EtOH added RuCl3 and excess p-mentha-1,5-diene; soln. refluxed under microwave irradiation for 15 min; after cooling to room temp. solvent removed under vac.; residue washed with ether, complex collected by filteration, washed withether and dried; elem. anal.;
RuCl3 treated with α-phellandrene in according with early published method (M.A. Bennet, G.B. Robertson, A.K. Smith, J. Organomet. Chem. 43 (1972) C41);
In dimethylsulfoxide soln. of ligand in DMSO and RuCl3 in 2:1 molar ratio was heated under reflux for 6 h; cooled; 2 M NaCl added; residue filtered off; washed (H2O); dried (air);elem. anal.;