反応 #1509586

反応方程式

2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile

POCl3

→

title compound

6-Chloro-2-methyl-nicotinonitrile

反応条件

後処理

1. 1
   温度was refluxed for 3 h
2. 2
   その他The reaction mixture was dried down in vacuum and ice
3. 3
   workup.ADDITIONwas added
4. 4
   抽出The aqueous layer was extracted with EtOAc
5. 5
   その他The organic layer was separated
6. 6
   その他dried
7. 7
   濃縮concentrated in vacuum

実験手順

A mixture of 2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile (44 g) and POCl3 (250 ml) was refluxed for 3 h. The reaction mixture was dried down in vacuum and ice followed by conc. aqueous ammonia (300 ml) was added. The aqueous layer was extracted with EtOAc. The organic layer was separated, dried and concentrated in vacuum affording the title compound (23.5 g, BP (18 mbar) 119-120° C.).

出典