反应详情

温度

75 °C

A suspension of 4-bromo-3,5-dimethylphenyl acetate (12.1 g, 49.8 mmol), N-bromosuccinimide (9.79 g, 55.0 mmol) and 2,2′-azobisisobutyronitrile (82.1 mg, 0.500 mmol) in carbon tetrachloride (100 mL) was stirred at 75° C. for 5 hr under nitrogen atmosphere. The reaction mixture was ice-cooled, and concentrated under reduced pressure. The residue was diluted with diethyl ether, the insoluble substance was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-25:75) to give the title compound (11.7 g, yield 73%) as colorless crystals.

1. temperaturecooled
2. concentrationconcentrated under reduced pressure
3. additionThe residue was diluted with diethyl ether
4. filtrationthe insoluble substance was filtered off
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-25:75)