HRID981539

反应详情

EQUATION

反应方程式

HRID 981539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4'-chloro-2-methyl-2-(1H-1,2,4-triazol-1-yl)propiophenone (1.375 g), trimethyl sulphoxonium iodide (1.6 g), aqueous sodium hydroxide (5N; 13.5 ml.), cetrimide (80 mg.) and 1,1,1-trichloroethane (30 ml.) was heated at 80° for 24 hours. The solution was cooled and diluted with methylene chloride (30 ml.), and the organic layer was separated and dried (MgSO4). Removal of the solvent, followed by flash chromatography of the residue on silica (100 g.) using ethyl acetate/hexane/diethylamine (40:60:3 v/v/v) for elution, gave, after collection of appropriate fractions and evaporation, the title oxirane as an oil in 79% yield, 1.15 g.

WORKUP

后处理

  1. temperaturewas heated at 80° for 24 hours
  2. temperatureThe solution was cooled
  3. customthe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. customRemoval of the solvent
  6. washfor elution
  7. customgave
  8. customafter collection of appropriate fractions and evaporation