反应详情

温度

200 °C

A mixture of 1-(3-bromo-5-chloro-2-hydroxy-4-methylphenyl)ethanone (4.85 g, 18.4 mmol) and copper cyanide (2.47 g, 27.6 mmol) in N-methylpyrrolidinone (15 mL) was heated at 200° C. for 1 hour. After cooling to room temperature, the mixture was diluted with ethyl acetate and 1 N HCl. The layers were separated and the aqeous layer was extracted with ethyl acetate. The combined organic layers were washed with water, then brine and dried over magnesium sulfate. After concentration to dryness under reduced pressure, the residue was used directly in the next step (3.7 g, 96%). LCMS calculated for C10H9ClNO2 (M+H)+: m/z=210.0; Found: 210.1.

1. temperatureAfter cooling to room temperature
2. customThe layers were separated
3. extractionthe aqeous layer was extracted with ethyl acetate
4. washThe combined organic layers were washed with water
5. dry with materialbrine and dried over magnesium sulfate
6. concentrationAfter concentration to dryness under reduced pressure