Реакция #2186243

ord-ee4b7bf01ddb48f4af3a8c774e0faa2e

Уравнение реакции

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

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураto cool down to room temperature
  2. 2
    Концентрированиеconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added chloroform and ice water
  4. 4
    Другоеwas separated to two layer
  5. 5
    ПромывкаThe organic layer was washed sequentially with water and saturated brine
  6. 6
    Сушкаdried over anhydrous sodium sulfate
  7. 7
    Концентрированиеconcentrated under reduced pressure

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07569518B2uspto-grants-2009_08