تفاعل #2186238
ord-0170c108a8204f028ed0f0cf1930e8e4
معادلة التفاعل
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
المردود 97.2%
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
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).