반응 #1509586

반응 방정식

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

POCl3

→

title compound

6-Chloro-2-methyl-nicotinonitrile

반응 조건

후처리

1. 1
   온도was refluxed for 3 h
2. 2
   기타The reaction mixture was dried down in vacuum and ice
3. 3
   workup.ADDITIONwas added
4. 4
   추출The aqueous layer was extracted with EtOAc
5. 5
   기타The organic layer was separated
6. 6
   기타dried
7. 7
   농축concentrated in vacuum

실험 절차

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.).

출처