HRID1701444

反应详情

EQUATION

反应方程式

HRID 1701444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium borohydride (1.24 g) in water (7 ml) was added to a solution of methyl 3α-hydroxy-11-oxo-5α-androstane-17β-carboxylate (2.58 g) in methanol (60 ml) and the mixture refluxed for 30 minutes. A further portion of sodium borohydride (200 mg) in a little water was added and refluxing continued for 10 minutes more. Most of the solvent was removed in vacuo and, after cooling, the crystalline product was collected by filtration. Recrystallization from aqueous methanol afforded title compound (1.662 g),

WORKUP

后处理

  1. temperaturethe mixture refluxed for 30 minutes
  2. temperaturerefluxing
  3. customMost of the solvent was removed in vacuo
  4. temperatureafter cooling
  5. filtrationthe crystalline product was collected by filtration
  6. customRecrystallization from aqueous methanol