HRID1457758

反应详情

EQUATION

反应方程式

HRID 1457758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 25 g (64 mmol) of 3-(5-chloro-2-methoxybenzamido)-2,2-dimethyl-7-methoxy-4-chromanone and 1.24 g (32 mmol) of powdered sodium borohydride in 100 ml of ethanol was stirred at 50° C. for 3 hours, during which the solid dissolved. After cooling, the solution was then poured into ice-water acidified with hydrochloric acid, and extracted with methylene chloride. The organic solution was washed with water, dried and evaporated. The resulting 3-(5-chloro-2-methoxybenzamido)-2,2-dimethyl-7-methoxy-4-chromanol (diastereomer mixture) melted from 165° C.

WORKUP

后处理

  1. dissolutiondissolved
  2. temperatureAfter cooling
  3. extractionextracted with methylene chloride
  4. washThe organic solution was washed with water
  5. customdried
  6. customevaporated
  7. custommelted from 165° C.