HRID542981

反应详情

EQUATION

反应方程式

HRID 542981 的结构方程式

PROCEDURE

实验过程

A suspension of 16.5 g. of 4'-amino-3',5'-dimethyl-2-(methylsulfonyl)-acetophenone and 10.6 g. of sodium borohydride in 500 ml. of alcohol was stirred at room temperature for 20 hours, resulting in a solution. After the addition of 500 ml. of water, the alcohol was evaporated under vacuum and the mixture was extracted with two 1 liter portions of ethyl acetate. The ethyl acetate extract was washed with two 500 ml. portions of water, dried over magnesium sulfate and evaporated under vacuum. After crystallization of the residue from ether, there was obtained 4-amino-3,5-dimethyl-α-[(methylsulfonyl)-methyl]-benzyl alcohol having a melting point of 146°-148° C.

WORKUP

后处理

  1. additionA suspension of 16.5 g
  2. customresulting in a solution
  3. additionAfter the addition of 500 ml
  4. customof water, the alcohol was evaporated under vacuum
  5. extractionthe mixture was extracted with two 1 liter portions of ethyl acetate
  6. extractionThe ethyl acetate extract
  7. washwas washed with two 500 ml
  8. dry with materialportions of water, dried over magnesium sulfate
  9. customevaporated under vacuum
  10. customAfter crystallization of the residue from ether