Reaktion #2186236

ord-3e15725fca184f6083058db8cc09b7bc

Reaktionsgleichung

Cc1n[nH]c(=O)c(-c2c(F)cccc2F)c1-c1ccc(Cl)cc1
5-(4-chlorophenyl)-4-(2,6-difluoropheyl)-6-methyl-2H-pyridazin-3-one
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1nnc(Cl)c(-c2c(F)cccc2F)c1-c1ccc(Cl)cc1
3-chloro-5-(4-chlorophenyl)-4-(2,6-difluorophenyl)-6-methyl pyridazine

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool down to room temperature
  2. 2
    Einengenconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added ethyl acetate and ice water
  4. 4
    Sonstigewas separated to two layer
  5. 5
    WaschenThe organic layer was washed sequentially with water and saturated brine
  6. 6
    Trocknendried over anhydrous sodium sulfate
  7. 7
    Einengenconcentrated under reduced pressure

Vorschrift

7.61 g of 5-(4-chlorophenyl)-4-(2,6-difluoropheyl)-6-methyl-2H-pyridazin-3-one and 40 ml of phosphorus oxychloride were mixed and stirred at 110° C. for 4 hours. There action mixture was allowed to cool 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 8.52 g of 3-chloro-5-(4-chlorophenyl)-4-(2,6-difluorophenyl)-6-methyl pyridazine (hereinafter, referred to as compound (xiv) of the present invention).

Quelle

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