反应详情

A refluxing solution of 2,6-dichloro-4-methylbenzophenone (3.44 g, 13.0 mmol) and dibenzoylperoxide (325 mg, 1.34 mmol) in benzene (130 ml) was treated in portions with N-bromosuccinimide (2.75 g, 15.5 mmol). After 3 hours at reflux, the mixture was cooled and evaporated under vacuum. The residue was triturated with diethyl ether (150 ml), filtered, and evaporated under vacuum. The residue was chromatographed on a column of silica gel (250 g) eluted with 4:1 (v/v) hexane-dichloromethane to provide 2.58 g (58%) 4-benzoyl-3,5-dichlorobenzyl bromide, m.p. 111°-113° C.

1. temperatureAfter 3 hours at reflux
2. temperaturethe mixture was cooled
3. customevaporated under vacuum
4. customThe residue was triturated with diethyl ether (150 ml)
5. filtrationfiltered
6. customevaporated under vacuum
7. customThe residue was chromatographed on a column of silica gel (250 g)
8. washeluted with 4:1 (v/v) hexane-dichloromethane