HRID2049478

反应详情

EQUATION

反应方程式

HRID 2049478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2β-Ethoxy-17,17-ethylenedioxy-3α-hydroxy-5α-androstan-11-one (8.2 g) was added to hydroxylamine hydrochloride (15 g) in ethanol (500 ml) containing 44% sodium hydroxide solution (90 ml). After refluxing for 24 hours about half the solvent was evaporated in vacuo and the residue was diluted with water and extracted with ethyl acetate. The washed and dried (Na2SO4) organic solution was evaporated in vacuo to afford a froth which on crystallization from ethyl acetate-petroleum ether afforded the title compound m.p. 136°-140°, [α]D +41.1°.

WORKUP

后处理

  1. temperatureAfter refluxing for 24 hours about half the solvent
  2. customwas evaporated in vacuo
  3. additionthe residue was diluted with water
  4. extractionextracted with ethyl acetate
  5. washThe washed
  6. dry with materialdried (Na2SO4) organic solution
  7. customwas evaporated in vacuo
  8. customto afford a froth which
  9. customon crystallization from ethyl acetate-petroleum ether