Phosphorus oxychloride → HCID 86680708, Verbindung

HRID 1500759Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1500759
[N+:1]([C:4]1[C:5](O)=[N:6][C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)=[N:8][CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][N:8]=[C:7]([C:10]2[CH:11]=[N:12][N:13]3[CH:18]=[CH:17][N:16]=[CH:15][C:14]=23)[N:6]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178526803HCID 178526803, Verbindung

Produkt 1

HCID 86680708HCID 86680708, VerbindungAusbeute 86 %

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A suspension of 5-nitro-2-(pyrazolo[1,5-a]pyrazin-3-yl)pyrimidin-4-ol (Preparation 24d, 1.50 g, 5.8 mmol) in phosphoryl trichloride (12 mL) was stirred and heated to 90° C. in a sealed tube. After 2 hours, the mixture was concentrated in vacuo and the residue was azeotroped with toluene. The resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution and, upon scratching, a solid formed which was filtered, washed with water (40 mL) and dried to give the title compound (1.38 g, 86%) as a yellow solid.

Aufarbeitung

  1. concentrationthe mixture was concentrated in vacuo
  2. customthe residue was azeotroped with toluene
  3. additionThe resultant solid was treated with saturated aqueous sodium hydrogen carbonate solution
  4. customa solid formed which
  5. filtrationwas filtered
  6. washwashed with water (40 mL)
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2b5986abc31b483b89c611ed400a19e9
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09206183B2

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