HRID1375001

反应详情

EQUATION

反应方程式

HRID 1375001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added to the mixture under nitrogen atmosphere
  2. customThe resulting precipitates
  3. filtrationwere filtered off
  4. washwashed with tetrahydrofuran
  5. customevaporated under reduced pressure
  6. customto give a crude oil
  7. customThe oil was purified by column chromatography on silica gel using
  8. additiona mixture of dichloromethane and methanol (40:1)