Reaktion #524944

Reaktionsgleichung

N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride

4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine

diethylamine hydrochloride

potassium carbonate

→

N,N-Diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine

Lösungsmittel

ethanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture containing 8.2 g
2. 2
   Einengenconcentrated in vacuo to dryness
3. 3
   Sonstigethe solid collected
4. 4
   workup.DISSOLUTIONThe solid was dissolved
5. 5
   workup.ADDITIONthe hot solution treated with decolorizing charcoal
6. 6
   Filtrationfiltered
7. 7
   Temperaturto cool
8. 8
   workup.ADDITIONsaturated with gaseous hydrogen chloride, ether was added to turbidity
9. 9
   SonstigeThe separated solid was collected
10. 10
    Sonstigedried in vacuo at 80° C.
11. 11
    Sonstigeto yield 7.4 g

Vorschrift

A mixture containing 8.2 g. of 4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine, 8.7 g. of diethylamine hydrochloride, 100 ml. of ethanol, 6 g. of potassium carbonate and 10 ml. of water was refluxed with stirring for eight hours and then concentrated in vacuo to dryness. The residue was swirled in water and the solid collected. The solid was dissolved in boiling isopropyl alcohol, the hot solution treated with decolorizing charcoal and filtered, and the hot filtrate allowed to cool. The filtrate was then saturated with gaseous hydrogen chloride, ether was added to turbidity and the mixture was allowed to stand. The separated solid was collected and dried in vacuo at 80° C. to yield 7.4 g. of N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride, m.p. 205°-208° C.

Quelle