Diisopropylethylamine → HCID 118383130, 화합물

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C[N:2](/[CH:4]=[C:5](/[C:16](=O)[C:17]([F:20])([F:19])[F:18])\[C:6]([O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:7])C.Cl.[NH:23]([CH:25]1[CH2:30][CH2:29][C:28]([CH2:32][C:33]([O:35][CH2:36][CH3:37])=[O:34])([CH3:31])[CH2:27][CH2:26]1)N.CCN(C(C)C)C(C)C>CCO>[CH2:36]([O:35][C:33](=[O:34])[CH2:32][C:28]1([CH3:31])[CH2:27][CH2:26][CH:25]([N:23]2[C:16]([C:17]([F:20])([F:19])[F:18])=[C:5]([C:6]([O:8][CH2:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[O:7])[CH:4]=[N:2]2)[CH2:30][CH2:29]1)[CH3:37]

참가 물질

실험 절차

A solution of (Z)-benzyl 2-((dimethylamino)methylene)-4,4,4-trifluoro-3-oxobutanoate (2.018 g, 6.70 mmol) in EtOH (20 mL) was added dropwise to a solution of ethyl 2-(4-hydrazinyl-1-methylcyclohexyl)acetate hydrochloride (1.6 g, 6.38 mmol) and DIPEA (2.452 ml, 14.04 mmol) in EtOH (31.9 ml) at ambient temperature. The reaction was allowed to stir overnight. The solvent was removed and the residual oil was purified using a 40 g REDISEP™ Gold SiO2 column eluting with 0-25% EtOAc/hexane using the Gold resolution method. Fractions containing the desired product were combined and concentrated in vacuo to provide benzyl 1-(4-(2-ethoxy-2-oxoethyl)-4-methylcyclohexyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (2.12 g, 4.69 mmol, 73.4% yield) as a mixture of isomers (colorless syrup). LCMS=453.4 (M+H)+.