Реакция #2186228

Уравнение реакции

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

Выход 82.8%

Условия реакции

Обработка

1. 1
   Температураto cool down to room temperature
2. 2
   Концентрированиеconcentrated under reduced pressure
3. 3
   workup.ADDITIONTo the residue was added ethyl acetate and ice water
4. 4
   Другоеseparated to two layer
5. 5
   ПромывкаThe organic layer was washed sequentially with water and saturated brine
6. 6
   Сушкаdried over anhydrous sodium sulfate
7. 7
   Концентрированиеconcentrated under reduced pressure

Методика

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).

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