反应详情

温度

80 °C

An ambient temperature solution of 2,6-dichloro-4-methylbenzoyl chloride (5.5 g, 25 mmol) in benzene (30 ml) was treated in portions with aluminum chloride (3.45 g, 25.9 mmol). When hydrogen chloride evolution ceased, the mixture was heated at 80° C. for 15 hours. The mixture was cooled, quenched by addition of ice and concentrated hydrochloric acid (5 ml), and diluted with diethyl ether (50 ml). The layers were separated and the organic phase washed with water, dried over anhydrous magnesium sulfate, and evaporated to dryness under vacuum. The semisolid residue was chromatographed on a column of silica gel (300 g) eluted with 4:1 (v/v) hexanedichloromethane to provide 4.60 g (69%) 2,6-dichloro-4-methylbenzophenone, m.p. 75.5°-76.5° C.

1. temperatureThe mixture was cooled
2. customquenched by addition of ice and concentrated hydrochloric acid (5 ml)
3. additiondiluted with diethyl ether (50 ml)
4. customThe layers were separated
5. washthe organic phase washed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated to dryness under vacuum
8. customThe semisolid residue was chromatographed on a column of silica gel (300 g)
9. washeluted with 4:1 (v/v) hexanedichloromethane