Reaktion #2186231

ord-7a87827e5e9441289425a161ab29226b

Reaktionsgleichung

Cc1n[nH]c(=O)c(-c2cc(F)cc(F)c2F)c1-c1ccc(Cl)cc1
5-(4-chlorophenyl)-6-methyl-4-(2,3,5-trifluorophenyl)-2H-pyridazin-3-one
O=P(Cl)(Cl)Cl
phosphorus oxychloride
Cc1nnc(Cl)c(-c2cc(F)cc(F)c2F)c1-c1ccc(Cl)cc1
3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,3,5-trifluorophenyl)pyridazine
Ausbeute 96.6%

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool down to room temperature
  2. 2
    Einengenconcentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added ethyl acetate and ice water
  4. 4
    Sonstigewas separated to two layer
  5. 5
    WaschenThe organic layer was washed sequentially with water and saturated brine
  6. 6
    Trocknendried over anhydrous sodium sulfate
  7. 7
    Einengenconcentrated under reduced pressure

Vorschrift

1.80 g of 5-(4-chlorophenyl)-6-methyl-4-(2,3,5-trifluorophenyl)-2H-pyridazin-3-one and 10 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, to obtain 1.83 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2,3,5-trifluorophenyl)pyridazine (hereinafter, referred to as compound (viii) of the present invention).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07569518B2uspto-grants-2009_08