HRID371062

反应详情

EQUATION

反应方程式

HRID 371062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (11β,17β)-17-(ethylthio)-9-fluoro-11-hydroxyandrosta-1,4-dien-3-one (700 mg, 1.92 mmole; see example 6) in chloroform (30 ml) was added a solution of 86% m-chloroperbenzoic acid (390 mg, 1.95 mmole) in chloroform (15 ml). An instantaneous reaction was noted (tlc). The solution was then washed with a 10% potassium carbonate solution and water, dried (anhydrous magnesium sulfate) and evaporated to afford the title compound (697 mg) as a solid. One crystallization of this from ethyl acetate followed by drying (100° C., 0.3 mm of Hg, 10 hours) gave the analytical specimen of the title compound (600 mg), melting point 247°-250° C., with consistent spectral data.

WORKUP

后处理

  1. customAn instantaneous reaction
  2. washThe solution was then washed with a 10% potassium carbonate solution and water
  3. dry with materialdried (anhydrous magnesium sulfate)
  4. customevaporated