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HRID1649471

反应详情

EQUATION

反应方程式

HRID 1649471 的结构方程式

REACTANTS

反应物

3
结构：ClCCl
HCID6344

Dichloromethane

CH2Cl2

结构：c1ccc(P(c2ccccc2)c2ccccc2)cc1
HCID11776

Triphenylphosphine

C18H15P

结构：C[C@]12CC[C@H]3[C@@H]([C@@H](O)[C@H]4O[C@]45C[C@@H](O[Si](Cc4ccccc4)(Cc4ccccc4)Cc4ccccc4)CC[C@]35C)[C@@H]1[C@@H]1C[C@@H]1C2=O
HCID88686820

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CC[C@H]3[C@@H]([C@H](Cl)[C@H]4O[C@]45C[C@@H](O[Si](Cc4ccccc4)(Cc4ccccc4)Cc4ccccc4)CC[C@]35C)[C@@H]1[C@@H]1C[C@@H]1C2=O
HCID88687372

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

结构：ClC(Cl)(Cl)Cl
溶剂HCID5943

Carbon tetrachloride

CCl4

PROCEDURE

实验过程

24 g of 3β-tribenzylsilyloxy-5,6β-epoxy-7β-hydroxy-15β,16β-methylene-5β-androstan-17-one is dissolved in a mixture of 250 ml of methylene chloride, 250 ml of carbon tetrachloride, and 125 ml of pyridine and stirred with 24 g of triphenylphosphine for 3 hours. The mixture is then washed with water, dried over sodium sulfate, and concentrated under vacuum. After chromatography on silica gel with hexane-acetone, 19.8 g of 3β-tribenzylsilyloxy-7α-chloro-5,6β-epoxy-15β,16β-methylene-5β-androstan-17-one is obtained.

WORKUP

后处理

  1. washThe mixture is then washed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under vacuum