HRID1837264

反应详情

EQUATION

反应方程式

HRID 1837264 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

5.0 g of 7α-(5-chloropentyl)-11β-fluoro-3-hydroxy-estra-1,3,5(10)-trien-17-one is dissolved in 100 ml of methanol and mixed in portions at 0° C. with 0.96 g of sodium borohydride. After 30 minutes of stirring at 0° C., the reaction mixture is added to semi-saturated sodium chloride solution, extracted 3 times with ethyl acetate and washed once with saturated common salt solution. After drying on magnesium sulfate, it is concentrated by evaporation in a vacuum. Preparative column chromatography on silica gel with a hexane-ethyl acetate gradient yields 4.29 g of 7α-(5-chloropentyl)-11β-fluor-estra-1,3,5(10)-triene-3,17β-diol.

WORKUP

后处理

  1. extractionextracted 3 times with ethyl acetate
  2. washwashed once with saturated common salt solution
  3. customAfter drying on magnesium sulfate, it
  4. concentrationis concentrated by evaporation in a vacuum