HRID1165509
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture is heated
- temperatureat reflux for 2.5 hours
- concentrationThe solution is then concentrated to a volume of 25 ml
- additiondiluted with trichloromethane
- washwashed with 5% hydrochloric acid, aqueous sodium bicarbonate, and brine
- concentrationConcentration and chromatography