تفاعل #2186244

ord-bfae9d0dcd8e4507880660d4940a4283

معادلة التفاعل

Cc1n[nH]c(=O)c(-c2c(F)cc(F)cc2F)c1-c1ccc(Cl)c(Cl)c1
5-(3,4-dichlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1nnc(Cl)c(-c2c(F)cc(F)cc2F)c1-c1ccc(Cl)c(Cl)c1
3-chloro-5-(3,4-dichlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

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

1.75 g of 5-(3,4-dichlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one and 6 ml 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 1.80 g of 3-chloro-5-(3,4-dichlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (xxiii) of the present invention).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07569518B2uspto-grants-2009_08