HRID1077162

反应详情

EQUATION

反应方程式

HRID 1077162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 13β-ethyl-3-methoxygona-1,3,5(10),8-tetraen-17-one (16.8 g.) to a solution of sodium borohydride (6 g.) in methanol (500 cc.), swirl the mixture which boils spontaneously. When all the material has been added and the reaction has subsided, add acetic acid (15 cc.). Reduce the mixture in volume by evaporation of most of the solvent, add water and extract the product with ether. Evapoate the washed and dried extracts to obtain crude crystalline product (16.8 g.), m.p. 102°-5° on recrystallization from acetonitrile.

WORKUP

后处理

  1. additionWhen all the material has been added
  2. customReduce the mixture in volume by evaporation of most of the solvent
  3. additionadd water
  4. extractionextract the product with ether
  5. washEvapoate the washed
  6. customdried extracts
  7. customto obtain crude crystalline product (16.8 g.), m.p. 102°-5°
  8. customon recrystallization from acetonitrile