반응 #2186226

ord-182c5c62e4784c12be36cc85d2e4e680

반응 방정식

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

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was cooled down to room temperature
  2. 2
    농축concentrated under reduced pressure
  3. 3
    workup.ADDITIONTo the residue was added ethyl acetate and ice water
  4. 4
    기타was separated to two layer
  5. 5
    세척The organic layer was washed sequentially with water and saturated brine
  6. 6
    건조dried over anhydrous sodium sulfate
  7. 7
    농축concentrated under reduced pressure

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07569518B2uspto-grants-2009_08