Phosphorus pentachloride → 7-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine

HRID 2417659Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2417659
[CH3:1][N:2]1[C:10]2[C:9](O)=[N:8][C:7]([CH3:12])=[N:6][C:5]=2[C:4]([CH3:13])=[N:3]1.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>P(Cl)(Cl)(Cl)=O>[Cl:15][C:9]1[C:10]2[N:2]([CH3:1])[N:3]=[C:4]([CH3:13])[C:5]=2[N:6]=[C:7]([CH3:12])[N:8]=1

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 178433418HCID 178433418, Verbindung

Produkt 1

HCID 133384077-Chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidineAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

A mixture of 30.5 g (0.17 mol) of 1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidin-7-ol and 37 g (0.18 mol) of phosphorus pentachloride in 350 ml of phosphorus oxychloride is stirred under reflux for seven hours and the resulting solution is evaporated in vacuo. The solid residue is redissolved in 300 ml of methylenedichloride and stirred with 200 ml of a saturated aqueous solution of sodium bicarbonate. The organic layer is dried over MgSO4 and evaporated in vacuo to give 30 g (98%) of 7-chloro-1,3,5-trimethyl-1H-pyrazolo[4,3-d]pyrimidine, mp 91°-93° C. from ethyl acetate-pet ether.

Aufarbeitung

  1. temperatureunder reflux for seven hours
  2. customthe resulting solution is evaporated in vacuo
  3. dissolutionThe solid residue is redissolved in 300 ml of methylenedichloride
  4. stirringstirred with 200 ml of a saturated aqueous solution of sodium bicarbonate
  5. dry with materialThe organic layer is dried over MgSO4
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b4185639f7834fcd95dd23cbffdf0b11
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04469868

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