huagongshe.com
HRID597357

反应详情

EQUATION

反应方程式

HRID 597357 的结构方程式

REACTANTS

反应物

2
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：CCC(=O)OC[C@]12CCC(=O)C=C1CC[C@@H]1[C@@H]2CC[C@]2(C)[C@@H](OC(=O)CC)CC[C@@H]12
HCID54342612

未命名化合物

PRODUCTS

生成物

1
结构：CCC(=O)O[C@H]1CC[C@H]2[C@@H]3CCC4=CC(=O)CC[C@]4(CO)[C@H]3CC[C@]12C
HCID54223287

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CO
溶剂HCID887

Methanol

CH4O

结构：O
溶剂HCID962

Water

H2O

2 次

PROCEDURE

实验过程

A solution of 11 g of 17β,19-bis(1-oxopropoxy)androst-4-en-3-one in 2 liters of methanol is treated with 2.5 g of sodium carbonate in 250 ml of water and refluxed for one hour after which the reaction mixture is poured into 10 liters of water, and the solid collected by filtration. The solid is dissolved in methylene chloride, dried over magnesium sulfate, filtered and the solvent removed. The residue is crystallized from acetone-hexane yielding 6 g of 19-hydroxy-17β(1-oxopropoxy)androst-4-en-3-one. M.P. 160°-162° C.

WORKUP

后处理

  1. temperaturerefluxed for one hour after which the reaction mixture
  2. filtrationthe solid collected by filtration
  3. dissolutionThe solid is dissolved in methylene chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent removed
  7. customThe residue is crystallized from acetone-hexane yielding 6 g of 19-hydroxy-17β(1-oxopropoxy)androst-4-en-3-one