Реакция #1509586
ord-7cdb17f067a04e22aa9305970d553803
Уравнение реакции
2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile
POCl3
→
title compound
6-Chloro-2-methyl-nicotinonitrile
Реагенты
Нет
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураwas refluxed for 3 h
- 2ДругоеThe reaction mixture was dried down in vacuum and ice
- 3workup.ADDITIONwas added
- 4ЭкстракцияThe aqueous layer was extracted with EtOAc
- 5ДругоеThe organic layer was separated
- 6Другоеdried
- 7Концентрированиеconcentrated in vacuum
Методика
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.).