Reaktion #2186236
ord-3e15725fca184f6083058db8cc09b7bc
Reaktionsgleichung
5-(4-chlorophenyl)-4-(2,6-difluoropheyl)-6-methyl-2H-pyridazin-3-one
phosphorus oxychloride
→
3-chloro-5-(4-chlorophenyl)-4-(2,6-difluorophenyl)-6-methyl pyridazine
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturto cool down to room temperature
- 2Einengenconcentrated under reduced pressure
- 3workup.ADDITIONTo the residue was added ethyl acetate and ice water
- 4Sonstigewas separated to two layer
- 5WaschenThe organic layer was washed sequentially with water and saturated brine
- 6Trocknendried over anhydrous sodium sulfate
- 7Einengenconcentrated 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).