huagongshe.com
HRID2254632

反应详情

EQUATION

反应方程式

HRID 2254632 的结构方程式

REACTANTS

反应物

4
结构：c1ccncc1
HCID1049

Pyridine

C5H5N

结构：COC(C)(C)OC
HCID6495

2,2-Dimethoxypropane

C5H12O2

结构：Cc1ccc(S(=O)(=O)[O-])cc1.c1cc[nH+]cc1
HCID466102

未命名化合物

结构：C[C@]12CCC(=O)C=C1CC[C@@H]1[C@@H]2[C@@H](F)C[C@]2(C)C(=O)CC[C@@H]12
HCID13990933

未命名化合物

PRODUCTS

生成物

1
结构：COC1=CC2=CC[C@@H]3[C@H]([C@@H](F)C[C@]4(C)C(=O)CC[C@@H]34)[C@@]2(C)CC1
HCID13990945

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

PROCEDURE

实验过程

10.0 g of 11β-fluoroandrost-4-ene-3,17-dione [U.S. Pat. No. 3,966,713 (1976)] is stirred under reflux with 60 ml of dimethoxypropane and 1.0 g of pyridinium-4-toluenesulfonate. After 8 hours, 1 ml of pyridine is added, the mixture is diluted with ethyl acetate, washed neutral with water, and dried. The crude product is chromatographed on silica gel with an acetone-hexane gradient. Yield: 7.8 g of 11β-fluoro-3-methoxyandrosta-3,5-diene-17-one as a foam.

WORKUP

后处理

  1. washwashed neutral with water
  2. customdried
  3. customThe crude product is chromatographed on silica gel with an acetone-hexane gradient