反应详情

温度

200 °C

A mixture of 1-(3-bromo-5-chloro-2-hydroxy-4-methylphenyl)ethanone (4.9 g, 18 mmol) and copper cyanide (2.5 g, 28 mmol) in N-methylpyrrolidinone (15 mL) was heated at 200° C. for 1 hour. The resulting mixture was allowed to cool to room temperature and was then diluted with ethyl acetate and 1 N HCl. The organic and aqueous layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried over magnesium sulfate and concentrated to dryness under reduced pressure to give 3-Acetyl-5-chloro-2-hydroxy-6-methylbenzonitrile (3.7 g, 96%). LCMS calculated for C10H9ClNO2 (M+H)+: m/z=210.0. found: 210.1.

1. temperatureto cool to room temperature
2. customThe organic and aqueous layers were separated
3. extractionthe aqueous layer was extracted with ethyl acetate
4. washThe combined organic layers were washed with water and brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated to dryness under reduced pressure