HRID1647641

反应详情

EQUATION

反应方程式

HRID 1647641 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 4.5 g of 14β,15β-epoxy-17β-(3-furyl)-5β-androstan-3-one in 30 ml of dry tetrahydrofuran at-78° C, a solution of 9.8 g of tri-tert-butoxyaluminum-hydride in tetrahydrofuran was added dropwise. The mixture was stirred for 20 hrs, then 40 ml of water were added and the temperature raised to 25° C. The aluminum salts were filtered on a celite cake and washed with methanol. The solution was concentrated under reduced pressure and extracted with methylene chloride. The organic layer was dried over sodium sulfate and evaporated to dryness under reduced pressure to give 4.3 g of the title compound (II-b) as a white solid.

WORKUP

后处理

  1. filtrationThe aluminum salts were filtered on a celite cake
  2. washwashed with methanol
  3. concentrationThe solution was concentrated under reduced pressure
  4. extractionextracted with methylene chloride
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customevaporated to dryness under reduced pressure