Phosphorus oxychloride → HCID 178508434, Verbindung

HRID 1982102Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1982102
[NH2:1][C:2]1[N:7]=[C:6]2[N:8]=[CH:9][CH:10]=[C:5]2[C:4](=O)[N:3]=1.P(Cl)(Cl)([Cl:14])=O>>[NH2:1][C:2]1[NH:7][C:6]2=[N:8][CH:9]=[CH:10][C:5]2=[C:4]([Cl:14])[N:3]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 219043482-Amino-4H-pyrrolo[2,3-d]pyrimidin-4-one

Produkt 1

HCID 178508434HCID 178508434, Verbindung

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

2-Aminopyrrolo[2,3-d]pyrimidin-4-one (45 g) was suspended in phosphorus oxychloride (150 ml) and the suspension was stirred at 110° C. for 3 hours. The excess amount of phosphorus oxychloride was distilled off under reduced pressure and ice water (600 ml) was added to the residue, whereby the residue was thoroughly dissolved. The solution was cooled with stirring and adjusted to pH 9 with concentrated aqueous ammonia. The resulting precipitate was collected by filtration, washed with water and recrystallized from hot methanol (4 l) to give the above-identified compound (34.6 g).

Aufarbeitung

  1. distillationThe excess amount of phosphorus oxychloride was distilled off under reduced pressure and ice water (600 ml)
  2. additionwas added to the residue, whereby the residue
  3. dissolutionwas thoroughly dissolved
  4. temperatureThe solution was cooled
  5. stirringwith stirring
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. customrecrystallized from hot methanol (4 l)

Quellen und Nachweise

ORD-Eintrag
ord-b3fd495a34da49408506d66f494a6cc9
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04595530

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