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

HRID 908615
ノート
印刷プレビュー

反応式

HRID 908615 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178517789HCID 178517789、化合物

生成物 1

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

実験手順

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).

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  • 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)
  • 出典と根拠

    ORDレコード
    ord-2e4c8bce905746708ca12f4f7119b058
    出典データセット
    uspto-grants-2011_09
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US08017612B2

    反応ノート

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