反应详情

温度

100 °C

To a solution of 4-cyano-2,3-difluoro-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide (0.693 g, 1.53 mmol) (Example I11) in dimethyl-sulfoxide (2.32 ml) was added ammonium carbonate (69 mg, 1.75 mmol). The reaction mixture was heated to 100° C. for 16 hours. The reaction mixture was allowed to cool to ambient temperature and then partitioned between water and ethyl acetate. The organic phase was dried over sodium sulfate and concentrated. The residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 7:3) to give 3-amino-4-cyano-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-2-fluorobenzamide (290 mg, 42% yield). 1H-NMR (400 MHz, CDCl3): 2.35 (6H, s), 4.68 (1H, bs), 7.35-7.41 (4H, m), 7.74 (1H, d) ppm.

1. temperatureto cool to ambient temperature
2. custompartitioned between water and ethyl acetate
3. dry with materialThe organic phase was dried over sodium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 7:3)