Reaktion #1509586

Reaktionsgleichung

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

POCl3

→

title compound

6-Chloro-2-methyl-nicotinonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 3 h
2. 2
   SonstigeThe reaction mixture was dried down in vacuum and ice
3. 3
   workup.ADDITIONwas added
4. 4
   ExtraktionThe aqueous layer was extracted with EtOAc
5. 5
   SonstigeThe organic layer was separated
6. 6
   Sonstigedried
7. 7
   Einengenconcentrated in vacuum

Vorschrift

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.).

Quelle