huagongshe.com
HRID855484

反应详情

EQUATION

反应方程式

HRID 855484 的结构方程式

REACTANTS

反应物

1
结构：C[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
HCID10193144

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1Cc2cc(O)ccc2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@@H]2F
HCID67201552

未命名化合物

收率 56.4%

AUXILIARIES

试剂、催化剂与溶剂

3
结构：[Br][Cu][Br]
催化剂HCID24611

Copper bromide (CuBr2)

Br2Cu

结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

A solution of 500 mg of 11β-fluoro-7α-methylestr-4-ene-3,17-dione in 16.5 ml of acetonitrile was stirred with 400 mg of copper(II) bromide for 6.5 hours at 25° C. Then, it was diluted with ethyl acetate, washed with sodium bicarbonate solution and sodium chloride solution, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with hexane/acetone. 280 mg of pure 11β-fluoro-3-hydroxy-7α-methylestra-1,3,5(10)-trien-17-one with a melting point of 185-186° C. was obtained.

WORKUP

后处理

  1. washwashed with sodium bicarbonate solution and sodium chloride solution
  2. customdried on sodium sulfate
  3. concentrationconcentrated by evaporation in a vacuum
  4. customchromatographed on silica gel with hexane/acetone