HRID441310

反应详情

EQUATION

反应方程式

HRID 441310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 7.4 g. of 3',5'-bis(dimethylamino)-2-methylsulfonylacetophenone and 3.8 g. of sodium borohydride in 100 ml. of ethanol was stirred for 20 hours at 25° C. After the addition of 50 ml. of water, the alcohol was removed in vacuo and the remaining aqueous suspension extracted with 400 ml. of ethyl acetate. The ethyl acetate phases were washed with 50 ml. of water, dried over magnesium sulfate and evaporated to dryness in vacuo. Recrystallization of the residue from ethanol gave 3,5-bis(dimethylamino)- α -[(methylsulfonyl)-methyl]-benzyl alcohol, having a melting point of 142°-143° C.

WORKUP

后处理

  1. additionA suspension of 7.4 g
  2. additionAfter the addition of 50 ml
  3. customof water, the alcohol was removed in vacuo
  4. extractionthe remaining aqueous suspension extracted with 400 ml
  5. washThe ethyl acetate phases were washed with 50 ml
  6. dry with materialof water, dried over magnesium sulfate
  7. customevaporated to dryness in vacuo
  8. customRecrystallization of the residue from ethanol