Reacción #1509586

ord-7cdb17f067a04e22aa9305970d553803

Ecuación de reacción

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

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas refluxed for 3 h
  2. 2
    OtroThe reaction mixture was dried down in vacuum and ice
  3. 3
    workup.ADDITIONwas added
  4. 4
    ExtracciónThe aqueous layer was extracted with EtOAc
  5. 5
    OtroThe organic layer was separated
  6. 6
    Otrodried
  7. 7
    Concentraciónconcentrated in vacuum

Procedimiento

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.).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: USRE045323E1uspto-grants-2015_01