Реакция #1509586

ord-7cdb17f067a04e22aa9305970d553803

Уравнение реакции

Cc1[nH]c(=O)ccc1C#N
2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile
O=P(Cl)(Cl)Cl
POCl3
Cc1nc(Cl)ccc1C#N
title compound
Cc1nc(Cl)ccc1C#N
6-Chloro-2-methyl-nicotinonitrile

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed for 3 h
  2. 2
    ДругоеThe reaction mixture was dried down in vacuum and ice
  3. 3
    workup.ADDITIONwas added
  4. 4
    ЭкстракцияThe aqueous layer was extracted with EtOAc
  5. 5
    ДругоеThe organic layer was separated
  6. 6
    Другоеdried
  7. 7
    Концентрированиеconcentrated 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.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE045323E1uspto-grants-2015_01