Реакция #2186238
ord-0170c108a8204f028ed0f0cf1930e8e4
Уравнение реакции
4-(2-chloro-6-fluorophenyl)-5-(4-chlorophenyl)-6-methyl-2H-pyridazin-3-one
phosphorus oxychloride
→
3-chloro-4-(2-chloro-6-fluorophenyl)-5-(4-chlorophenyl)-6-methylpyridazine
Выход 97.2%
Реактанты
Реагенты
Нет
Условия реакции
Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Температураto cool down to room temperature
- 2Концентрированиеconcentrated under reduced pressure
- 3workup.ADDITIONTo the residue was added ethyl acetate and ice water
- 4Другоеwas separated to two layer
- 5ПромывкаThe organic layer was washed sequentially with water and saturated brine
- 6Сушкаdried over anhydrous sodium sulfate
- 7Концентрированиеconcentrated under reduced pressure
Методика
2.16 g of 4-(2-chloro-6-fluorophenyl)-5-(4-chlorophenyl)-6-methyl-2H-pyridazin-3-one and 10 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 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 2.21 g of 3-chloro-4-(2-chloro-6-fluorophenyl)-5-(4-chlorophenyl)-6-methylpyridazine (hereinafter, referred to as compound (xvi) of the present invention).