HRID651947

反应详情

EQUATION

反应方程式

HRID 651947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25-Hydroxycholesterol (3.4 gms) and dichlorodicyanoquinone (6.5 gms) dissolved in purified dioxan (100 mls) were heated at reflux for 20 hrs. The mixture was filtered and the solvent evaporated. Chromatography of the residue on alumina and elution with ethyl acetate and benzene afforded the trienone. Recrystallization from methanol gave the title compound, melting point 183°-184°. νmax. 3600, 1650 and 1600 cm-1.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureat reflux for 20 hrs
  3. filtrationThe mixture was filtered
  4. customthe solvent evaporated
  5. washChromatography of the residue on alumina and elution with ethyl acetate and benzene
  6. customafforded the trienone
  7. customRecrystallization from methanol