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HRID1606343

反应详情

EQUATION

反应方程式

HRID 1606343 的结构方程式

REACTANTS

反应物

3
结构：CC(=O)O
HCID176

Acetic Acid

C2H4O2

结构：CCN(CC)CC
HCID8471

Triethylamine

C6H15N

结构：CO[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
HCID86733284

未命名化合物

PRODUCTS

生成物

1
结构：CO[C@H]1C[C@@]2(C)[C@@H](CC[C@H]3[C@@H]4CC[C@H](C(=O)COC(C)=O)[C@@]4(C)CC(=O)[C@@H]32)C[C@@H]1O
HCID86733285

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

结构：ClC(Cl)Cl
溶剂HCID6212

Chloroform

CHCl3

PROCEDURE

实验过程

21-Bromo-3α-hydroxy-2β-methoxy-5α-pregnane-11,20-dione (600 mg.) was dissolved in dry acetone (15 ml.) and added to a mixture of glacial acetic acid (2 ml.) and triethylamine (3ml.) and refluxed for 41/2 hours. The mixture was diluted with chloroform, washed with water, dried and evaporated to a foam. Purification by preparative tlc followed by crystallisation from ethyl acetate and petrol gave the title compound (230 mg.) as colourless plates; m.p. 177°-180° [α]D + 112°.

WORKUP

后处理

  1. temperaturerefluxed for 41/2 hours
  2. washwashed with water
  3. customdried
  4. customevaporated to a foam
  5. customPurification by preparative tlc
  6. customfollowed by crystallisation from ethyl acetate and petrol