تفاعل #2186229

معادلة التفاعل

5-(4-chlorophenyl)-4-(2,6-difluoro-4-ethoxyphenyl)-6-methyl-2H-pyridazin-3-one

phosphorus oxychloride

→

3-chloro-5-(4-chlorophenyl)-4-(2,6-difluoro-4-ethoxyphenyl)-6-methylpyridazine

المردود 61.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool down to room temperature
2. 2
   تركيزconcentrated under reduced pressure
3. 3
   workup.ADDITIONTo the residue was added ethyl acetate and ice water
4. 4
   أخرىwas separated to two layer
5. 5
   غسيلThe organic layer was washed sequentially with water and saturated brine
6. 6
   تجفيفdried over anhydrous sodium sulfate
7. 7
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

0.25 g of 5-(4-chlorophenyl)-4-(2,6-difluoro-4-ethoxyphenyl)-6-methyl-2H-pyridazin-3-one and 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 under reduced pressure. The residue was subjected to preparative thin layer chromatography (stationary phase: silica gel, developing solvent: hexane/ethyl acetate=3/1), to obtain 0.16 g of 3-chloro-5-(4-chlorophenyl)-4-(2,6-difluoro-4-ethoxyphenyl)-6-methylpyridazine (hereinafter, referred to as compound (vi) of the present invention).

المصدر