HRID2099866

反应详情

EQUATION

反应方程式

HRID 2099866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Water (50 ml) was added to a solution of (2α,3α,5α,16β,17β)2,3-epoxy-16-(1-pyrrolidinyl)-androstan-17-ol (85.2 g) in morpholine (500 ml) and the reaction mixture was heated at reflux temperature for 3 d. Evaporation of the reaction mixture gave a crude product, which was crystallised from acetone. Recrystallisation from methanol gave pure (2β,3α,5α,16β,17β)-2(4-morpholinyl)-16-(1-pyrro lidinyl)-androstane-3,17-diol (71.2 g), m.p. 212°-219° C.; [α]D20=+87.9° (c 1.02 in CHCl3).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux temperature for 3 d
  3. customEvaporation of the reaction mixture
  4. customgave a crude product, which
  5. customwas crystallised from acetone
  6. customRecrystallisation from methanol