Diisopropylcarbodiimide → 2-(2,6-Dichloro-phenylamino)-6-fluoro-1-methyl-1h-benzimidazole-5-carboxylic acid
反応式
CC(C)N=C=NC(C)C.C([O:12][C:13](=[O:35])[C:14]1[CH:19]=[C:18]([NH:20][C:21]([NH:23][C:24]2[C:29]([Cl:30])=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:31])=S)[C:17]([NH:32][CH3:33])=[CH:16][C:15]=1[F:34])C>C(#N)C>[Cl:30][C:29]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:31])[C:24]=1[NH:23][C:21]1[N:32]([CH3:33])[C:17]2[CH:16]=[C:15]([F:34])[C:14]([C:13]([OH:12])=[O:35])=[CH:19][C:18]=2[N:20]=1参加物
4
実験手順
DIC (1.50 mL, 9.6 mmol) was added to a stirred mixture of 5-[3-(2,6-dichloro-phenyl)-thioureido]-2-fluoro-4-methylamino-benzoic acid ethyl ester (2.70 g, 6.5 mmol) in acetonitrile. After stirring for 1 h the mixture was concentrated i.vac. The residue was taken up in ethanol and 1 M aq. NaOH and stirred for further 40 min at reflux. Ethanol was evaporated, the mixture was diluted with water and filtered. The filtrate was acidified with hydrochloric acid, stirred and filtered. Both residues were combined and dried.