反应详情

A solution of 4-cyano-2,5-difluoro-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-3-nitro-benzamide (5.99 g, 12 mmol) (Example I16) in methanol was reacted with hydrogen for 16 hours in the presence of 10% palladium on carbon (40 bar, 40° C.). The reaction mixture was filtered to remove the catalyst and the filtrate concentrated. The residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 7:3) to give 3-amino-4-cyano-2,5-difluoro-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide (0.953 g, 17% yield). 1H-NMR (400 MHz, CDCl3): 2.36 (6H, s), 4.82 (2H, bs), 7.12 (1H, m), 7.38 (2H, s), 7.78 (1H, d) ppm.

1. filtrationThe reaction mixture was filtered
2. customto remove the catalyst
3. concentrationthe filtrate concentrated
4. customThe residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 7:3)