تفاعل #2186236
ord-3e15725fca184f6083058db8cc09b7bc
معادلة التفاعل
5-(4-chlorophenyl)-4-(2,6-difluoropheyl)-6-methyl-2H-pyridazin-3-one
phosphorus oxychloride
→
3-chloro-5-(4-chlorophenyl)-4-(2,6-difluorophenyl)-6-methyl pyridazine
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةto cool down to room temperature
- 2تركيزconcentrated under reduced pressure
- 3workup.ADDITIONTo the residue was added ethyl acetate and ice water
- 4أخرىwas separated to two layer
- 5غسيلThe organic layer was washed sequentially with water and saturated brine
- 6تجفيفdried over anhydrous sodium sulfate
- 7تركيزconcentrated under reduced pressure
الإجراء التجريبي
7.61 g of 5-(4-chlorophenyl)-4-(2,6-difluoropheyl)-6-methyl-2H-pyridazin-3-one and 40 ml of phosphorus oxychloride were mixed and stirred at 110° C. for 4 hours. 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 8.52 g of 3-chloro-5-(4-chlorophenyl)-4-(2,6-difluorophenyl)-6-methyl pyridazine (hereinafter, referred to as compound (xiv) of the present invention).