Reaktion #2186235

Reaktionsgleichung

5-(4-chlorophenyl)-4-(2,5-difluorophenyl)-6-methyl-2H-pyridazin-3-one

phosphorus oxychloride

→

3-chloro-5-(4-chlorophenyl)-4-(2,5-difluorophenyl)-6-methyl pyridazine

Ausbeute 95.7%

Reaktionsbedingungen

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
8. 8
   Waschenelution solvent

Vorschrift

2.86 g of 5-(4-chlorophenyl)-4-(2,5-difluorophenyl)-6-methyl-2H-pyridazin-3-one and 6.5 g of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. The reaction 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. The residue was subjected to silica gel column chromatography (elution solvent; hexane:ethyl acetate=3:1, to obtain 2.89 g of 3-chloro-5-(4-chlorophenyl)-4-(2,5-difluorophenyl)-6-methyl pyridazine (hereinafter, referred to as compound (xiii) of the present invention).

Quelle