Reaktion #2186228

Reaktionsgleichung

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

phosphorus oxychloride

→

3-chloro-5-(4-chlorophenyl)-4-(2,6-difluoro-4-methoxyphenyl)-6-methylpyridazine

Ausbeute 82.8%

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
   Sonstigeseparated 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

185 mg of 5-(4-chlorophenyl)-4-(2,6-difluoro-4-methoxyphenyl)-6-methyl-2H-pyridazin-3-one and 5 g of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. 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 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. The residue was subjected to preparative thin layer chromatography (stationary phase: silica gel, developing solvent: hexane/ethyl acetate=3/1), to obtain 161 mg of 3-chloro-5-(4-chlorophenyl)-4-(2,6-difluoro-4-methoxyphenyl)-6-methylpyridazine (hereinafter, referred to as compound (v) of the present invention).

Quelle