HRID1076271

反应详情

EQUATION

反应方程式

HRID 1076271 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

0.70 g. of 2-methoxy-1,3,5 (10)-estratriene-3,17β-diol is heated under reflux and nitrogen purging in 10 ml. of toluene with 18 ml. of diisobutylaluminum hydride (20% in toluene) for 22 hours. The reaction mixture is cooled to about 0° C. and then decomposed with 5 ml. of ethanol and then with 5 ml. of ethanol-water mixture (1:1). The mixture is further worked up as set forth in Example 3. After purification from methanol, 0.45 g. of 1,3,5(10)-estratriene-2,3,17β-triol is obtained; m.p. 181°-183° C.; ε286 = 3420.

WORKUP

后处理

  1. temperatureunder reflux
  2. customAfter purification from methanol, 0.45 g