HRID1613967

反应详情

EQUATION

反应方程式

HRID 1613967 的结构方程式

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

  1. temperatureat reflux temperature
  2. temperatureAfter 24 hours of refluxing the reaction
  3. concentrationwas concentrated under reduced pressure
  4. customto give a solid, which
  5. customwas purified by column chromatography (silica gel; methylene chloride/diethyl ether 1/1)