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Phosphorus oxychloride → 4-Chloro-2-methylthio-6-(3-trifluoromethyl-phenyl)-pyrimidine

HRID 2053091
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반응식

HRID 2053091 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7](O)[CH:6]=[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)[N:4]=1.P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:7]1[CH:6]=[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)[N:4]=[C:3]([S:2][CH3:1])[N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 1785035332-methylsulfanyl-6-[3-(trifluoromethyl)phenyl]-1H-pyrimidin-4-one

생성물 1

HCID 866125004-Chloro-2-methylthio-6-(3-trifluoromethyl-phenyl)-pyrimidine

실험 절차

2-Methylsulfanyl-6-(3-trifluoromethyl-phenyl)-pyrimidin-4-ol (2.11 g) was heated to reflux in phosphorous oxychloride (15 mL) for four hours. Phosphorous oxychloride was evaporated under reduced pressure and the remaining residue dissolved in ethyl acetate (100 mL) and washed with saturated sodium chloride (50 mL). Organics were separated, dried over sodium sulphate and solvent was evaporated under reduced pressure to yield product 4-chloro-2-methylsulfanyl-6-(3-trifluoromethyl-phenyl)-pyrimidine (2.11 g) as a brown oil.

후처리

  1. customPhosphorous oxychloride was evaporated under reduced pressure
  2. dissolution
the remaining residue dissolved in ethyl acetate (100 mL)
  • washwashed with saturated sodium chloride (50 mL)
  • customOrganics were separated
  • dry with materialdried over sodium sulphate and solvent
  • customwas evaporated under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-0e288497c0384273830aca8dcbdd0cf6
    출처 데이터셋
    uspto-grants-2008_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07326715B2

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