Реакция #2186227
ord-8b50f1e8c2c446c7b427d852bb073744
Уравнение реакции
5-(4-chlorophenyl)-6-methyl-4-(2,3,6-trifluorophenyl)-2H-pyridazin-3-one
phosphorus oxychloride
→
3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,3,6-trifluorophenyl)pyridazine
Выход 99.9%
Реактанты
Реагенты
Нет
Условия реакции
Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ТемператураThe reaction mixture was cooled 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
3.50 g of 5-(4-chlorophenyl)-6-methyl-4-(2,3,6-trifluorophenyl)-2H-pyridazin-3-one and 15 g of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. The reaction mixture was cooled 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 3.68 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,3,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (iv) of the present invention).