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Phosphorus oxychloride → 2-chloro-7-[3-(trifluoromethyl)pyridin-2-yl]-N-[5-(trifluoromethyl) pyridin-2-yl]-[1,8]naphthyridin-4-amine

HRID 1724842
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반응식

HRID 1724842 반응식
[F:1][C:2]([F:32])([F:31])[C:3]1[C:4]([C:9]2[N:18]=[C:17]3[C:12]([C:13]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][N:22]=4)=[CH:14][C:15](O)=[N:16]3)=[CH:11][CH:10]=2)=[N:5][CH:6]=[CH:7][CH:8]=1.P(Cl)(Cl)([Cl:35])=O>>[Cl:35][C:15]1[CH:14]=[C:13]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][N:22]=2)[C:12]2[C:17](=[N:18][C:9]([C:4]3[C:3]([C:2]([F:32])([F:31])[F:1])=[CH:8][CH:7]=[CH:6][N:5]=3)=[CH:10][CH:11]=2)[N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178516409HCID 178516409, 화합물

생성물 1

HCID 575611422-chloro-7-[3-(trifluoromethyl)pyridin-2-yl]-N-[5-(trifluoromethyl) pyridin-2-yl]-[1,8]naphthyridin-4-amine

실험 절차

Heat 7-[3-(trifluoromethyl)pyridin-2-yl]-4-{[5-(trifluoromethyl)pyridin-2-yl]amino}-[1,8]naphthyridin-2-ol (112 mg) and phosphorus oxychloride (1 mL) at reflux for 1 hour. Evaporate to dryness, partition between ethyl acetate and saturated aqueous NaHCO3 and extract with EtOAc. Dry the combined organics over Na2SO4, concentrate under vacuum to obtain the title compound.

후처리

  1. temperatureat reflux for 1 hour
  2. customEvaporate to dryness
  3. custompartition between ethyl acetate and saturated aqueous NaHCO3
  • extractionextract with EtOAc
  • dry with materialDry the combined organics over Na2SO4
  • concentrationconcentrate under vacuum
  • 출처 및 근거

    ORD 기록
    ord-ce3901480faa4588900d52cfcf7c94b6
    출처 데이터셋
    uspto-grants-2009_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07488740B2

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