Reacción #88236

ord-ebac018909a54f20af991c206b66b15b

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroat the ambient temperature
  2. 2
    TemperaturaThe reaction mixture was refluxed for 12 hours
  3. 3
    OtroThe organic layer was separated
  4. 4
    Lavadowashed with water and brine
  5. 5
    Secadodried over sodium sulfate
  6. 6
    OtroThe solvent was evaporated

Procedimiento

The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09440968B2uspto-grants-2016_09