HRID1613967
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 3,3-ethylenedioxy-9α-hydroxyandrost-5-en-17-one (3.46 g) in nitromethane (75 ml) under a nitrogen atmosphere 1,2-diaminoethane (0.1 ml) was added at reflux temperature. After 24 hours of refluxing the reaction was almost complete as measured by TLC. After cooling to room temperature the reaction mixture was concentrated under reduced pressure to give a solid, which was purified by column chromatography (silica gel; methylene chloride/diethyl ether 1/1) to provide the title compound.
WORKUP
后处理
- temperatureat reflux temperature
- temperatureAfter 24 hours of refluxing the reaction
- concentrationwas concentrated under reduced pressure
- customto give a solid, which
- customwas purified by column chromatography (silica gel; methylene chloride/diethyl ether 1/1)