HRID2670

反应详情

EQUATION

反应方程式

HRID 2670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 100 mg. (0.303 mmol) of 3-acetoxy-androst-5-en-17-one in 3 ml EtOH at -10° C., was added 22.9 mg (0.606 mmol) of sodium borohydride with stirring. After the reaction mixture was stirred for one and 1/2 hours, the mixture was diluted with 10 ml water, the ethanol solvent removed under vacuum, and the residue extracted with ethyl acetate. The organic layer was washed with aqueous Na2CO3, brine, dried over sodium sulfate and concentrated to leave a residue of crude title compound. Proton NMR confirmed the assigned structure.

WORKUP

后处理

  1. stirringAfter the reaction mixture was stirred for one and 1/2 hours
  2. customthe ethanol solvent removed under vacuum
  3. extractionthe residue extracted with ethyl acetate
  4. washThe organic layer was washed with aqueous Na2CO3, brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated