HRID1838892

反应详情

EQUATION

反应方程式

HRID 1838892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.77 g of 11β-fluoro-7x-[5-(methylamino)-pentyl]oestra-1,3,5(10)-triene-3,17β-diol in 18 ml of dimethylformamide is stirred at a bath temperature of 80° C. for 1 hour with 1.4 g of 8,8,9,9,9-penta-fluorononyl tosylate. The mixture is then added to water, extracted 3 times with ethyl acetate, washed with water and sodium chloride solution, dried over sodium sulphate, concentrated in vacuo and the residue is chromatographed on silica gel using dichloromethane/methanol. 11β-Fluoro-7α-{5-[methyl(8,8,9,9,9-penta-fluorononyl)amino]pentyl}oestra-1,3,5(10)-triene-3,17β-diol is obtained as crystals of melting point 11° C.

WORKUP

后处理

  1. extractionextracted 3 times with ethyl acetate
  2. washwashed with water and sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue is chromatographed on silica gel