Phosphorus oxychloride → 7-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

HRID 573345Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 573345
[CH2:1]([N:3]1[C:11]2[C:10](O)=[N:9][CH:8]=[N:7][C:6]=2[CH:5]=[N:4]1)[CH3:2].O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:10]1[C:11]2[N:3]([CH2:1][CH3:2])[N:4]=[CH:5][C:6]=2[N:7]=[CH:8][N:9]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 178463033HCID 178463033, Verbindung

Produkt 1

HCID 714458087-Chloro-1-ethyl-1H-pyrazolo[4,3-d]pyrimidine

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 1-ethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol (2.91 g) and POCl3 (30 mL) was stirred at 100° C. overnight. The mixture was concentrated under reduced pressure. The residue was neutralized with saturated NaHCO3 aqueous solution and extracted with AcOEt. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (2.14 g).

Aufarbeitung

  1. concentrationThe mixture was concentrated under reduced pressure
  2. extractionextracted with AcOEt
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-dfa8156422914e4a99cd25b0ab75f904
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029536B2

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