反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Lithium aluminum hydride (4.53 g) was added by small portions to an ice-cooled solution of 3-methoxy-4-(trifluoromethyl)benzoic acid (23.3 g) in tetrahydrofuran (400 ml) under nitrogen atmosphere, and the mixture was stirred at room temperature for 2 hours. After being cooled with ice, 2N sodium hydroxide (2 ml) was added to the mixture under nitrogen atmosphere. The resulting precipitates were filtered off and washed with tetrahydrofuran, and the filtrate and washings were combined and evaporated under reduced pressure to give a crude oil. The oil was purified by column chromatography on silica gel using a mixture of dichloromethane and methanol (40:1) to give 3-methoxy-4-(trifluoromethyl)benzyl alcohol (20 g) as a colorless oil.
WORKUP
后处理
- additionwas added to the mixture under nitrogen atmosphere
- customThe resulting precipitates
- filtrationwere filtered off
- washwashed with tetrahydrofuran
- customevaporated under reduced pressure
- customto give a crude oil
- customThe oil was purified by column chromatography on silica gel using
- additiona mixture of dichloromethane and methanol (40:1)