HRID848782

反应详情

EQUATION

反应方程式

HRID 848782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chlorine in acetic acid (0.84 M, 12 ml.) is added dropwise with stirring to 17β-methoxy-5α-androstan-3-one (3.0 g.) in acetic acid (10 ml.). When the addition is complete the reaction mixture is chilled, and the precipitate which forms is filtered off, washed with water, dried and recrystallized from acetone-methylene chloride to give the title compound, m.p. 202°-210°; MS (m/e) 338, 306, 302, 291 and 265; NMR (CDCl3) 0.77, 1.10, 3.20, 3.30 and 4.06 δ.

WORKUP

后处理

  1. additionWhen the addition
  2. temperatureis chilled
  3. filtrationthe precipitate which forms is filtered off
  4. washwashed with water
  5. customdried
  6. customrecrystallized from acetone-methylene chloride