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HRID1576791

反应详情

EQUATION

反应方程式

HRID 1576791 的结构方程式

REACTANTS

反应物

2
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)[C@@H](C)C[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86733283

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H]1C[C@@]2(C)[C@@H](CC[C@H]3[C@@H]4CC[C@H](C(=O)CBr)[C@@]4(C)CC(=O)[C@@H]32)C[C@@H]1O
HCID131710459

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 solution of 3α-hydroxy-2β-methyl-5α-pregnane-11,20-dione (1.04g.) in dry methanol (150ml) was stirred at 0°-5° during the dropwise addition of a solution of bromine (0.16ml) in dry methanol (20ml) over a period of 2.5 hours. The reaction mixture was partitioned between ethyl acetate and water and the organic layer was separated, washed with water, dried (MgSO4) and evaporated to a white foam; purification by preparative t.l.c. (ethyl acetate: benzene 1:2.5) gave the title compound (510mg.), m.p. 140° dec.; [α]D + 133° (c 0.95).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. customthe organic layer was separated
  3. washwashed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated to a white foam
  6. custompurification by preparative t.l.c