Reaktion #82525

Reaktionsgleichung

2-amino-4-chloro-6-methylpyrimidine

ammonia

→

2,4-diamino-6-methylpyrimidine

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis placed in a high pressure vessel
2. 2
   Temperaturheated to 130°-165° C. under a pressure of 140-250 psig, where it
3. 3
   Sonstigethe reaction mixture is removed
4. 4
   WaschenThe reaction vessel is washed with 200 mL of methanol
5. 5
   EinengenThe combination is concentrated under reduced pressure to a residual solid
6. 6
   workup.STIRRINGThe solid is then stirred for 2 hours at ambient temperature with 100 mL of aqueous 30% ammonia
7. 7
   TemperaturThe mixture is cooled to 0° C.
8. 8
   Filtrationthe solid is collected by filtration
9. 9
   SonstigeThe solid is dried

Vorschrift

A mixture of 50.0 grams (0.348 mole) of 2-amino-4-chloro-6-methylpyrimidine (commercially available) and 100 mL of aqueous 30% ammonia in 400 mL of methanol is placed in a high pressure vessel and heated to 130°-165° C. under a pressure of 140-250 psig, where it is stirred for 13 hours. After this time, the reaction mixture is allowed to cool to ambient temperature. The reaction vessel is then opened and the reaction mixture is removed. The reaction vessel is washed with 200 mL of methanol, and the wash is combined with the reaction mixture. The combination is concentrated under reduced pressure to a residual solid. The solid is then stirred for 2 hours at ambient temperature with 100 mL of aqueous 30% ammonia. The mixture is cooled to 0° C., and the solid is collected by filtration. The solid is dried, yielding 40.8 grams of 2,4-diamino-6-methylpyrimidine. The NMR spectrum is consistent with the proposed structure.

Quelle