Реакция #2186235

Уравнение реакции

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

Выход 95.7%

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
   Другоеwas separated 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
8. 8
   Промывкаelution solvent

Методика

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).

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