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HRID1390740

反应详情

EQUATION

反应方程式

HRID 1390740 的结构方程式

REACTANTS

反应物

2
结构：CC(=O)O
HCID176

Acetic Acid

C2H4O2

结构：C[C@]12CC[C@H]3[C@@H](CCC4=CC(=O)[C@H]5C[C@H]5[C@@]43CO)[C@@H]1CCC2=O
HCID70605896

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1CC(=O)C=C2CC[C@@H]3[C@H](CC[C@]4(C)C(=O)CC[C@@H]34)[C@]21CO
HCID54279369

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Zn]
催化剂HCID23994

Zinc

Zn

结构：c1ccccc1
溶剂HCID241

Benzene

C6H6

PROCEDURE

实验过程

19-Hydroxy-1β,2β-methylene-4-androstene-3,17-dione, zinc powder, and acetic acid are heated to their reflux temperature for a period of about 1 hour. Upon cooling of the reaction mixture, benzene is added and the resulting suspension filtered. The filtrate is evaporated to dryness under vacuum and the residue remaining is chromatographed on a silica gel column and eluted with methylenechloride. The eluate is evaporated to dryness and the residue is crystallized from an acetone-hexane solution to yield 19-hydroxy-1β-methyl-4-androstene-3,17-dione.

WORKUP

后处理

  1. temperaturereflux temperature for a period of about 1 hour
  2. additionis added
  3. filtrationthe resulting suspension filtered
  4. customThe filtrate is evaporated to dryness under vacuum
  5. customthe residue remaining is chromatographed on a silica gel column
  6. washeluted with methylenechloride
  7. customThe eluate is evaporated to dryness
  8. customthe residue is crystallized from an acetone-hexane solution