HRID63265

反应详情

EQUATION

反应方程式

HRID 63265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-ethylpyridine (Commercial, e.g. Sigma-Aldrich) (10.7 g), ammonium peroxydisulfate (45.6 g) and concentrated sulphuric acid (4.5 ml) in methanol (150 ml)/water (70 ml) was refluxed for 24 h. The reaction mixture was slowly added onto aqueous sodium bicarbonate and extracted with chloroform (4×500 ml). This was dried over sodium sulphate, concentrated in vacuo and purified through silica using 0-60% ethyl acetate in hexane to give the title compound, 1.16 g Mass Spec: [MH]+=138.0

WORKUP

后处理

  1. extractionextracted with chloroform (4×500 ml)
  2. dry with materialThis was dried over sodium sulphate
  3. concentrationconcentrated in vacuo
  4. custompurified through silica using 0-60% ethyl acetate in hexane