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Water → 2,7-Dichloro-5-trifluoromethyl-thiazolo[4,5-d]pyrimidine

HRID 908615
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HRID 908615 반응식
[Cl:1][C:2]1[S:3][C:4]2[C:9](O)=[N:8][C:7]([C:11]([F:14])([F:13])[F:12])=[N:6][C:5]=2[N:15]=1.O.P(Cl)(Cl)([Cl:19])=O>>[Cl:1][C:2]1[S:3][C:4]2[C:9]([Cl:19])=[N:8][C:7]([C:11]([F:14])([F:13])[F:12])=[N:6][C:5]=2[N:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178517789HCID 178517789, 화합물

생성물 1

HCID 597038262,7-Dichloro-5-trifluoromethyl-thiazolo[4,5-d]pyrimidine

실험 절차

To a solution of the compound (1.35 g) obtained in Step 7 in phosphorus oxychloride (20 ml) was added water (190 mg) with stirring under ice-cooling, and the mixture was stirred at 100° C. for 3 hr. The reaction mixture was concentrated under reduced pressure, and partitioned by adding chloroform and water. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:10) to give the title compound (1.17 g).

후처리

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  • temperaturecooling
  • stirringthe mixture was stirred at 100° C. for 3 hr
  • concentrationThe reaction mixture was concentrated under reduced pressure
  • custompartitioned
  • additionby adding chloroform and water
  • washThe organic layer was washed successively with water and saturated brine
  • dry with materialdried over anhydrous magnesium sulfate
  • filtrationfiltrated
  • concentrationconcentrated under reduced pressure
  • customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:10)
  • 출처 및 근거

    ORD 기록
    ord-2e4c8bce905746708ca12f4f7119b058
    출처 데이터셋
    uspto-grants-2011_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08017612B2

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