[CH3:1][O:2][C:3]([C:5]1[CH:6]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[Cl:29])[C:7]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:8]([CH2:12][O:13][CH2:14][CH:15]=[N:16]O)[NH:9][C:10]=1[CH3:11])=[O:4].C([O-])=O.[NH4+]>CO.[OH-].[OH-].[Pd+2]>[CH3:1][O:2][C:3]([C:5]1[CH:6]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[Cl:29])[C:7]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[C:8]([CH2:12][O:13][CH2:14][CH2:15][NH2:16])[NH:9][C:10]=1[CH3:11])=[O:4]A mixture of 4-(2-chlorophenyl)-2-(2-hydroxyimino-ethoxymethyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylic acid 3-ethyl 5-methyl ester (IBa, 150 mg), palladium hydroxide on carbon (10 mg) and ammonium formate (224 mg) in methanol (10 mL) was refluxed for 5 h under a nitrogen atmosphere. On cooling to room temperature, the mixture was filtered through a pad of celite. The filtrate was concentrated in vacuo. Purification of the residue by flash chromatography on silica gel (grade 9385, Merck, 230-400 mesh, 60 Å) using a solvent mixture of dichloromethane and methanol (9:1; 100 mL), and dichloromethane, methanol and ammonium hydroxide (90:10:1; 500 mL) as eluent afforded the title compound (IAa 88 mg).
불러오는 중…
