تفاعل #2186243

ord-ee4b7bf01ddb48f4af3a8c774e0faa2e

معادلة التفاعل

Cc1ccc(-c2c(C)n[nH]c(=O)c2-c2c(F)cc(F)cc2F)cc1
6-methyl-5-(4-methylphenyl)-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1ccc(-c2c(C)nnc(Cl)c2-c2c(F)cc(F)cc2F)cc1
3-chloro-6-methyl-5-(4-methylphenyl)-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 chloroform 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

19.77 g of 6-methyl-5-(4-methylphenyl)-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one and 100 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 chloroform 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 19.90 g of 3-chloro-6-methyl-5-(4-methylphenyl)-4-(2,4,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (xxii) of the present invention).

المصدر

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