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

HRID 908615
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 908615
[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
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Komponenten

4

Edukt 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178517789HCID 178517789, Verbindung

Produkt 1

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

Versuchsvorschrift

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).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-2e4c8bce905746708ca12f4f7119b058
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08017612B2

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