反应详情

温度

140 °C

To a solution of 3-amino-4-cyano-N-[2,6-dimethyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-2-fluoro-benzamide (68 mg, 0.15 mmol) (Example I12) in tetrahydrofuran (2 ml) were added pyridine (36 μl, 0.45 mmol) and benzoyl chloride (21 μl, 0.18 mmol). The reaction mixture was heated in a microwave at 140° C. for 30 minutes. The reaction mixture was allowed to cool to ambient temperature. A second portion of benzoyl chloride (21 μl, 0.18 mmol) was added and heating repeated at 140° C. for 30 minutes. The reaction mixture was allowed to cool to ambient temperature and then partitioned between sodium hydrogen carbonate (1M) and ethyl acetate. The aqueous phase was extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated. The residue was purified by reverse-phase chromatography (eluent: trifluoroacetic acid/water/acetonitrile 1:4:5 to 1:1:8) to give Compound No. D15 of Table D (0.024 g, 28% yield). 1H-NMR (400 MHz, CDCl3): 2.28 (6H, s), 7.33 (2H, s), 7.45-7.96 (9H, m) ppm.

1. temperatureto cool to ambient temperature
2. temperatureheating
3. temperatureto cool to ambient temperature
4. custompartitioned between sodium hydrogen carbonate (1M) and ethyl acetate
5. extractionThe aqueous phase was extracted twice with ethyl acetate
6. dry with materialThe combined organic phases were dried over sodium sulfate
7. concentrationconcentrated
8. customThe residue was purified by reverse-phase chromatography (eluent: trifluoroacetic acid/water/acetonitrile 1:4:5 to 1:1:8)
9. customto give Compound No