反应详情

温度

50 °C

A suspension of 1-(4-cyclopropylmethoxy-2-methyl-phenyl)-ethanone from example A24 (6.4 g, 31.3 mmol) and N-bromosuccinimide (6.20 g, 34.5 mmol) in dry dimethylformamide (50 mL) is heated for 3 h at 50° C. After cooling to ambient temperature, water (200 mL) is added and the mixture is extracted with ethyl acetate (3×60 mL). The combined organic extracts are dried over sodium sulfate. The solvent is removed under reduced pressure. The crude is purified by column chromatography on silica gel using dichloromethane as eluent to give the title compound as a off-white solid. Yield: 4.80 g.

1. temperatureAfter cooling to ambient temperature
2. extractionthe mixture is extracted with ethyl acetate (3×60 mL)
3. dry with materialThe combined organic extracts are dried over sodium sulfate
4. customThe solvent is removed under reduced pressure
5. customThe crude is purified by column chromatography on silica gel