HRID1077171

反应详情

EQUATION

反应方程式

HRID 1077171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 13β-ethyl-3-methoxy-gona-1,3,5(10),8-tetraen-17β-ol (16.8 g.) dissolved in a mixture of aniline (150 cc.) and tetrahydrofuran (50 cc.) add liquid ammonia (400 cc.). Add lithium metal (6.0 g.) gradually in small pieces during 10 minutes, and stir the blue suspension obtained. After 2 hours, add ammonium chloride (50 g.) to the reaction mixture until a clear solution is obtained; then add water (600 cc.) and ether-extract the mixture. Evaporated the washed and dried extracts to obtain as residue a crystalline solid. Recrystallize from hexane (300 cc.), to obtain 13β-ethyl-3-methoxy-gona-1,3,5(10)-trien-17β-ol (14 g.), m.p. 126°-30°.

WORKUP

后处理

  1. customobtained
  2. customis obtained
  3. extractionthen add water (600 cc.) and ether-extract the mixture
  4. customEvaporated the
  5. washwashed
  6. customdried extracts
  7. customto obtain as residue a crystalline solid
  8. customRecrystallize from hexane (300 cc.)