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HRID918054

反应详情

EQUATION

反应方程式

HRID 918054 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：BrBr
HCID24408

Bromine

Br2

结构：CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID92786

Allopregnan-3α-ol-20-one

C21H34O2

PRODUCTS

生成物

1
结构：C[C@]12CC[C@@H](O)C[C@@H]1CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](C(=O)CBr)CC[C@@H]12
HCID54498956

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CO
溶剂HCID887

Methanol

CH4O

2 次

PROCEDURE

实验过程

A stirred solution of 3α-hydroxy-5α-pregnan-20-one (5 g., 15.7 mmole) in AR methanol (350 c.c.) was treated at 0° with a solution of bromine (1 c.c.) in methanol (23 c.c.) at such a rate that the yellow colour disappeared before further addition. The resultant suspension was poured into water and stirred for 30 minutes, and the precipitate was collected by filtration and dried in vacuo. The product was purified by column chromatography on silica gel MFC, (700 g.). Elution with benzene:ethyl acetate, 1:1) gave 21-bromo-3α-hydroxy-5α-pregnan-20-one (5.2 g.) [α]D + 105.5°.

WORKUP

后处理

  1. additiondisappeared before further addition
  2. filtrationthe precipitate was collected by filtration
  3. customdried in vacuo
  4. customThe product was purified by column chromatography on silica gel MFC, (700 g.)
  5. washElution with benzene