Reacción #2186226

ord-182c5c62e4784c12be36cc85d2e4e680

Condiciones de reacción

Temperatura
110°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture was cooled down to room temperature
  2. 2
    Concentraciónconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added ethyl acetate and ice water
  4. 4
    Otrowas separated to two layer
  5. 5
    LavadoThe organic layer was washed sequentially with water and saturated brine
  6. 6
    Secadodried over anhydrous sodium sulfate
  7. 7
    Concentraciónconcentrated under reduced pressure

Procedimiento

4.00 g of 5-(4-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one and 20 ml of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. The reaction mixture was cooled down to room temperature and concentrated under reduced pressure. To the residue was added ethyl acetate and ice water, and was separated to two layer. The organic layer was washed sequentially with water and saturated brine, and dried over anhydrous sodium sulfate, then, concentrated under reduced pressure, to obtain 4.16 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (i) of the present invention).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07569518B2uspto-grants-2009_08