Reaktion #55503

Reaktionsgleichung

sodium hydroxide

2,4-diamino-6-chloropyrimidine-3-oxide

o-xylene

1,2,5,6-tetrahydropyridine

→

2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is then heated
2. 2
   Temperaturto reflux for 30 minutes
3. 3
   Sonstigerising from 115° C. to 123° C
4. 4
   workup.ADDITIONtreated with 40 g
5. 5
   SonstigeThe precipitate formed
6. 6
   Filtrationis filtered off
7. 7
   Waschenwashed with 200 ml
8. 8
   Sonstigeof water and recrystallized from 3000 ml

Vorschrift

155 g. of 2,4-diamino-6-chloropyrimidine-3-oxide are mixed and stirred under an argon atmosphere with 640 ml. of o-xylene and 260 ml. of 1,2,5,6-tetrahydropyridine. The mixture is then heated to reflux for 30 minutes, the internal temperature rising from 115° C. to 123° C. The mixture is then cooled to 5° C., treated with 40 g. of sodium hydroxide in 400 ml. of water and stirred at 5° C. for 1 hour. The precipitate formed is filtered off, washed with 200 ml. of water and recrystallized from 3000 ml. of water, there being obtained pure 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide having a melting point of 263°-265° C. (decomposition).

Quelle