Reaction #2186226

ord-182c5c62e4784c12be36cc85d2e4e680

Conditions

Temperature
110°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07569518B2uspto-grants-2009_08