HRID2052256

反应详情

EQUATION

反应方程式

HRID 2052256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.38 gm. of sodium metal dissolved in 120 ml. of ethanol is added 6 ml. of 4-chlorobenzylmercaptan followed by 2.26 gm. of 17β-methanesulfonyloxy-1,4-androstadiene-3,11-dione. Heat at reflux for 96 hours. Obtain a residue in a manner similar to that described in Example 1A. Dissolve the residue in a minimum amount of chloroform and pass through a 200 gm. silica gel column. Elute with chloroform following the fractions by TLC. Combine the fractions, reduce, and crystallize the residue from ethyl acetate/hexane to obtain the title compound; m.p. 176°-180° C.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux for 96 hours
  3. customObtain a residue in a manner similar to
  4. washElute with chloroform following the fractions by TLC
  5. customcrystallize the residue from ethyl acetate/hexane