反应详情

Lithium aluminium hydride (400 mg, 10.4 mmol) was added in portions to a stirred solution of 2,6-dichloro-4-nitrobenzoyl chloride (3.0 g, 11.8 mmol) in diethyl ether (50 cm3) at room temperature. After 1.5 h the mixture was poured onto ice (80 g), acidified with 10% sulphuric acid (80 cm3) and extracted with ethyl acetate (3×60 cm3). The dried organic extracts were evaporated to an oil which was purified by chromatography over silica gel with a methanol-dichloromethane solvent gradient. The fractions containing 2,6-dichloro-4-nitrobenzylalcohol, were combined and evaporated under reduced pressure to a give a cream solid mp 111°-4° C. (0.7 g).

1. additionAfter 1.5 h the mixture was poured onto ice (80 g)
2. extractionextracted with ethyl acetate (3×60 cm3)
3. customThe dried organic extracts were evaporated to an oil which
4. customwas purified by chromatography over silica gel with a methanol-dichloromethane solvent gradient
5. additionThe fractions containing 2,6-dichloro-4-nitrobenzylalcohol
6. customevaporated under reduced pressure to