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HRID1834975

反应详情

EQUATION

反应方程式

HRID 1834975 的结构方程式

REACTANTS

反应物

2
结构：C[C@]12CC[C@H]3[C@@H](CC=C4C[C@@H](O)[C@H]5C[C@H]5[C@@]43C)[C@@H]1CC[C@@H]2O
HCID56628685

未命名化合物

结构：CC(C)=O.O=S(=O)(O)O.[O]=[Cr](=[O])=[O]
HCID131709961

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@]12C(=CC(=O)[C@H]3C[C@H]31)CC[C@@H]1[C@@H]2CC[C@]2(C)C(=O)CC[C@@H]12
HCID54262378

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

PROCEDURE

实验过程

1β,2β-Methylene-5-androstene-3β,17β-diol is dissolved in acetone and Jones reagent is added until a persistent yellow orange color appears. After stirring at room temperature for 10 minutes the mixture is poured onto icewater. The precipitate is collected by filtration and dissolved in a solution of sodium methoxide in methanol. Stirring is continued for about 30 minutes at room temperature, the methanol is removed and the residue triturated with water. The solid is filtered and crystallized from acetone to yield 1β,2β-methylene-4-androstene-3,17-dione.

WORKUP

后处理

  1. additionis poured onto icewater
  2. filtrationThe precipitate is collected by filtration
  3. dissolutiondissolved in a solution of sodium methoxide in methanol
  4. stirringStirring
  5. waitis continued for about 30 minutes at room temperature
  6. customthe methanol is removed
  7. customthe residue triturated with water
  8. filtrationThe solid is filtered
  9. customcrystallized from acetone