反应详情

温度

70 °C

N-(5-Cyano-2-fluoro-4-methoxybiphenyl-3-yl)-2,2,2-trifluoroacetamide 233) (2.78 g, 8.22 mmol) was dissolved in methanol (31.8 ml), and at room temperature, aqueous 15 wt. % potassium carbonate solution (31.8 ml, 34.5 mmol) was added. This was stirred at 70° C. for 38 hours. After cooling to room temperature, methanol was evaporated away under reduced pressure, and the resulting residue was extracted with ethyl acetate. The organic layer was separated, and the aqueous layer was again extracted with ethyl acetate. The organic layers were combined, washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=4:1) to obtain the entitled compound (1.833 g, 92%) as a colorless gel substance.

1. temperatureAfter cooling to room temperature
2. custommethanol was evaporated away under reduced pressure
3. extractionthe resulting residue was extracted with ethyl acetate
4. customThe organic layer was separated
5. extractionthe aqueous layer was again extracted with ethyl acetate
6. washwashed with saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. customThe solvent was evaporated away
9. customthe resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=4:1)