Реакция #2186226

ord-182c5c62e4784c12be36cc85d2e4e680

Уравнение реакции

Cc1n[nH]c(=O)c(-c2c(F)cc(F)cc2F)c1-c1ccc(Cl)cc1
5-(4-chlorophenyl)-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)cc1
3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine

Условия реакции

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

Обработка

  1. 1
    ТемператураThe reaction mixture was cooled down to room temperature
  2. 2
    Концентрированиеconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added ethyl acetate 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

4.00 g of 5-(4-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)-2H-pyridazin-3-one and 20 ml of phosphorus oxychloride were mixed and stirred at 110° C. for 1 hour. The reaction mixture was cooled 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 4.16 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,4,6-trifluorophenyl)pyridazine (hereinafter, referred to as compound (i) of the present invention).

Источник

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