HRID371053

反应详情

EQUATION

反应方程式

HRID 371053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1.7 g of (11β,17β)-9-Fluoro-11-hydroxy-17-mercaptoandrosta-1,4-dien-3-one dissolved in 100 ml of methanol, there was added 1 g of sodium hydroxide followed by 2.5 ml of allyl bromide (nitrogen atmosphere). The alkylation was complete after 1 hour of stirring at room temperature. The solution was partly evaporated, water was added and the resulting solid filtered and washed with water. Crystallization of the solid from ethyl acetate-petroleum ether furnished 1.08 g of the analytical sample, melting point 173°-175° C.

WORKUP

后处理

  1. customThe solution was partly evaporated
  2. additionwater was added
  3. filtrationthe resulting solid filtered
  4. washwashed with water
  5. customCrystallization of the solid from ethyl acetate-petroleum ether
  6. customfurnished 1.08 g of the analytical sample, melting point 173°-175° C.