Phosphorus pentachloride → 1H-Pyrazolo[4,3-d]pyrimidine, 7-chloro-1,3-dimethyl-5-(1-methylethyl)-

HRID 2417671Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2417671
[CH3:1][N:2]1[C:10]2[C:9](O)=[N:8][C:7]([CH:12]([CH3:14])[CH3:13])=[N:6][C:5]=2[C:4]([CH3:15])=[N:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:17]>P(Cl)(Cl)(Cl)=O>[Cl:17][C:9]1[C:10]2[N:2]([CH3:1])[N:3]=[C:4]([CH3:15])[C:5]=2[N:6]=[C:7]([CH:12]([CH3:14])[CH3:13])[N:8]=1

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 178433984HCID 178433984, Verbindung

Produkt 1

HCID 140065561H-Pyrazolo[4,3-d]pyrimidine, 7-chloro-1,3-dimethyl-5-(1-methylethyl)-Ausbeute 97,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

A mixture of 10 g (0.048 mol) of 1,3-dimethyl-5-isopropyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol and 10.2 g (0.049 mol) of phosphorus pentachloride in 70 ml of phosphorus oxychloride is stirred under reflux five hours and evaporated in vacuo. The residue is dissolved in 150 ml of methylene dichloride and stirred with 100 ml of a saturated solution of sodium bicarbonate. The organic layer is separated, dried over MgSO4, and evaporated in vacuo to to give 10.5 g of 7-chloro-1,3-dimethyl-5-isopropyl-1H-pyrazolo[4,3-d]pyrimidine, mp 87°-89° C. from pet ether.

Aufarbeitung

  1. temperatureunder reflux five hours
  2. customevaporated in vacuo
  3. dissolutionThe residue is dissolved in 150 ml of methylene dichloride
  4. stirringstirred with 100 ml of a saturated solution of sodium bicarbonate
  5. customThe organic layer is separated
  6. dry with materialdried over MgSO4
  7. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-93e5149f6ab841788b93b07fb3b08038
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04469868

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