反应 #1509586

反应方程式

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

POCl3

→

title compound

6-Chloro-2-methyl-nicotinonitrile

反应条件

后处理

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

实验过程

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.).

来源