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HRID918053

反应详情

EQUATION

反应方程式

HRID 918053 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]1[C@H](C)C[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3C(=O)C[C@@]21C
HCID70583911

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1C[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3C(=O)C[C@]2(C)[C@H]1C(=O)CBr
HCID131710389

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

3α-Hydroxy-16α-methyl-5α-pregnane-11,20-dione (5 g.) was dissolved in dry methanol (350 ml.) and treated at 0° with a solution of bromine (1 ml.) in dry methanol (24 ml.) at such a rate that the yellow colour disappeared before further addition. After completion of the addition the mixture was poured into water. The precipitated product was dried and dissolved in chloroform (20 ml.) and put onto a column of silica gel MFC (700 g.). Elution with benzene:ethyl acetate (21/2:1) gave the title compound (3.6 g.) as a foam, [α]D + 112.4°.

WORKUP

后处理

  1. additiondisappeared before further addition
  2. additionAfter completion of the addition the mixture
  3. customThe precipitated product was dried
  4. dissolutiondissolved in chloroform (20 ml.)
  5. washElution with benzene:ethyl acetate (21/2:1)