huagongshe.com
HRID1838882

反应详情

EQUATION

反应方程式

HRID 1838882 的结构方程式

REACTANTS

反应物

3
结构：[Br-].[Li+]
HCID82050

Lithium bromide

BrLi

结构：O=C([O-])O.[Na+]
HCID516892

Sodium Bicarbonate

CHNaO3

结构：CC(=O)OCCCCC[C@@H]1CC2=CC(=O)CC[C@@H]2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@@H]2F
HCID69935327

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)OCCCCC[C@@H]1Cc2cc(O)ccc2[C@H]2C(F)C[C@]3(C)C(=O)CC[C@H]3[C@H]12
HCID69936345

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Br][Cu][Br]
催化剂HCID24611

Copper bromide (CuBr2)

Br2Cu

结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

18.6 g of copper(II) bromide and 3.6 g of lithium bromide are added at 80° C. to 16.5 g of 7α-(5-acetoxy-pentyl)-11β-fluorooestr-4-ene-3,17-dione in 190 ml of acetonitrile. After 15 min, the reaction mixture is stirred into ice-water containing sodium hydrogen-carbonate. The precipitated product is filtered off with suction, dissolved in ethyl acetate, and the solution is washed with water, dried and concentrated in vacuo. After chromatographing the crude product on silica gel using a hexane-ethyl acetate gradient, 8.5 g of 7α-(5-acetoxypentyl)-11β-fluoro-3-hydroxyoestra-1,3,5(10)-trien-17-one are obtained as a foam.

WORKUP

后处理

  1. filtrationThe precipitated product is filtered off with suction
  2. dissolutiondissolved in ethyl acetate
  3. washthe solution is washed with water
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customare obtained as a foam