HRID1707906

反应详情

EQUATION

反应方程式

HRID 1707906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 10 g of 4-(4'-cyano-4-biphenylyl)cyclohexanone, 30 ml of diethyl ether and 270 ml of methanol was treated portionwise at 0° C. with 1.8 g of sodium borohydride. After 3 hours the reaction mixture was made acid (pH 1-2) with 25% hydrochloric acid. The reaction mixture was extracted three times with 50 ml of dichloromethane each time. The combined organic phases were washed twice with 500 ml of water each time and subsequently dried over magnesium sulfate, filtered and concentrated. Recrystallization from methanol gave 3.5 g of trans-4-(4'-cyano-4-biphenylyl)cyclohexanol.

WORKUP

后处理

  1. extractionThe reaction mixture was extracted three times with 50 ml of dichloromethane each time
  2. washThe combined organic phases were washed twice with 500 ml of water each time
  3. dry with materialsubsequently dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customRecrystallization from methanol