反应详情

Bromine (2 ml.) was added dropwise to a solution of p-chloro-2-(p-chlorophenyl)acetophenone (10 g.; 0.038 mole), chloroform (50 ml.) and diethyl ether (25 ml.). The mixture was heated at reflux for 0.5 hours and cooled (ca. 20°). Following a thorough washing with saturated sodium bicarbonate, the organic solution was dried over sodium sulfate and concentrated in vacuo. The residue was chromatographed at low pressure through silica gel 60 mesh (230-400) with 5% ethyl acetate in hexane. Recrystallization from hexane afforded 2.69 g.; m.p. 81.5°-83°.

1. temperatureThe mixture was heated
2. temperatureat reflux for 0.5 hours
3. temperaturecooled (ca. 20°)
4. washa thorough washing with saturated sodium bicarbonate
5. dry with materialthe organic solution was dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed at low pressure through silica gel 60 mesh (230-400) with 5% ethyl acetate in hexane
8. customRecrystallization from hexane
9. customafforded 2.69 g