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HRID371829

反应详情

EQUATION

反应方程式

HRID 371829 的结构方程式

REACTANTS

反应物

1
结构：C[C@H]1CC2(C=C3CC[C@H]4[C@@H]5CC[C@H](O)[C@@]5(C)CC[C@@H]4[C@]31CO)OCCS2
HCID22797424

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H]1CCC=C2CC[C@H]3[C@@H]4CC[C@H](O)[C@@]4(C)CC[C@@H]3[C@]21CO
HCID70584758

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Ni]
催化剂HCID935

Nickel

Ni

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

Raney nickel is added to a solution of 17β,19-dihydroxy-1α-methyl-4-androsten-3-one 3-ethylenethioketal in methanol and the resulting suspension is refluxed for 4 hours with rapid stirring. The suspension is cooled, filtered and the solvent evaporated. The remaining residue is chromatographed on silica gel an eluted with methylenechloride. Recrystallization from acetone-hexane yields the compound 1α-methyl-4-androstene-17β,19-diol.

WORKUP

后处理

  1. temperaturethe resulting suspension is refluxed for 4 hours with rapid stirring
  2. temperatureThe suspension is cooled
  3. filtrationfiltered
  4. customthe solvent evaporated
  5. customThe remaining residue is chromatographed on silica gel
  6. washan eluted with methylenechloride
  7. customRecrystallization from acetone-hexane