反应 #91543

ord-a37bdc801ed24874919533c44e84e722

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with chloroform (4×500 ml)
  2. 2
    干燥This was dried over sodium sulphate
  3. 3
    浓缩concentrated in vacuo
  4. 4
    其他purified through silica using 0-60% ethyl acetate in hexane

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

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09447074B2uspto-grants-2016_09