反応 #91543

反応方程式

4-ethylpyridine

ammonium peroxydisulfate

sulphuric acid

sodium bicarbonate

→

title compound

(4-ethyl-2-pyridinyl)methanol

溶媒

methanol

water

反応条件

後処理

1. 1
   抽出extracted with chloroform (4×500 ml)
2. 2
   乾燥This was dried over sodium sulphate
3. 3
   濃縮concentrated in vacuo
4. 4
   その他purified through silica using 0-60% ethyl acetate in hexane

実験手順

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

出典