HRID1165509

反应详情

EQUATION

反应方程式

HRID 1165509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of androst-5,7-diene-3β,17β-diol (2.9 g, 10 mmol) in 150 ml toluene is azeotropically dried for one hour. Butanone (15 ml) is added followed by aluminum isopropoxide (1.7 g,8 mmol) and the mixture is heated at reflux for 2.5 hours. The solution is then concentrated to a volume of 25 ml, diluted with trichloromethane, and washed with 5% hydrochloric acid, aqueous sodium bicarbonate, and brine. Concentration and chromatography affords androst-4,7-diene-3,17-dione.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 2.5 hours
  3. concentrationThe solution is then concentrated to a volume of 25 ml
  4. additiondiluted with trichloromethane
  5. washwashed with 5% hydrochloric acid, aqueous sodium bicarbonate, and brine
  6. concentrationConcentration and chromatography