反应详情

A mixture of methyl 3-methoxy-4-methylbenzoate (10.0 g, 55.5 mmol), N-bromosuccinimide (10.7 g, 60.9 mmol), 2,2′-azobis(isobutyronitrile) (1.6 mg) and ethyl acetate (200 ml) was heated under reflux overnight. The solvent was evaporated under reduced pressure, and hexane was added to the residue. The precipitate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (9:1-7:3, v/v) to give the title compound (12.8 g, 92%) as a colorless oil.

1. temperaturewas heated
2. temperatureunder reflux overnight
3. customThe solvent was evaporated under reduced pressure, and hexane
4. additionwas added to the residue
5. filtrationThe precipitate was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure
7. washeluted with hexane-ethyl acetate (9:1-7:3