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HRID900680

反应详情

EQUATION

反应方程式

HRID 900680 的结构方程式

REACTANTS

反应物

2
结构：[K+].[OH-]
HCID14797

Potassium hydroxide

HKO

结构：CC(=O)O[C@@H]1C[C@]2(C)C(=O)CC[C@H]2[C@H]2[C@H]1[C@H]1CCC(=O)C=C1C[C@H]2C
HCID12020272

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1CC2=CC(=O)CC[C@@H]2[C@@H]2[C@@H]1[C@@H]1CCC(=O)[C@@]1(C)C[C@H]2O
HCID12020273

未命名化合物

收率 100%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

PROCEDURE

实验过程

A solution of 1 g of 11α-acetoxy-7α-methyl-estr-4-ene-3,17-dione (E) in 20 ml of a 0.2 molar methanolic potassium hydroxide solution was stirred at room temperature for 3 hours. Then, it was added to water, extracted three times with ethyl acetate, washed neutral, dried on sodium sulfate, concentrated by evaporation in a vacuum and recrystallized from diethyl ether/acetone. 878 mg of pure 11α-hydroxy-7α-methyl-estr-4-ene-3,17-dione (F) with a melting point of 202.3° C. was obtained ([α]D20=+44.8° (c=0.5% in chloroform)).

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. washwashed neutral
  3. customdried on sodium sulfate
  4. concentrationconcentrated by evaporation in a vacuum
  5. customrecrystallized from diethyl ether/acetone