反应详情

A mixture of 6-acetyl-4-chloro-3′,5′-difluoro-3-methylbiphenyl-2-carbonitrile (0.20 g, 0.65 mmol) and potassium hydroxide (0.074 g, 1.3 mmol) in ethanol (0.9 mL) was refluxed for 2 hours. After cooled, the mixture was acidified with 1 N HCl and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, and evaporated to dryness under reduced pressure. The crude mixture was purified on silica gel, eluting with 0 to 80% ethyl acetate in hexane, to yield the desired product (61 mg, 29%). LCMS calculated for C16H13ClF2NO2 (M+H)+: m/z=324.1. found: 324.0.

1. temperaturewas refluxed for 2 hours
2. temperatureAfter cooled
3. extractionextracted with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over magnesium sulfate
6. customevaporated to dryness under reduced pressure
7. customThe crude mixture was purified on silica gel
8. washeluting with 0 to 80% ethyl acetate in hexane