Reaktion #10010

Reaktionsgleichung

2-chloro-9-ethyl-6-(3-cyano-phenyl-amino)-9H-purine

→

2-(2-Amino-ethyl-amino)-6-(3-cyano-phenyl-amino)-9-ethyl-9H-purine hydrochloride

Lösungsmittel

ethylenediamine

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto cool
2. 2
   WaschenThe organic phase is washed with water
3. 3
   Sonstigeseparated off
4. 4
   Trocknendried over sodium sulfate
5. 5
   SonstigeAfter removal of the solvent
6. 6
   workup.DISSOLUTIONthe residue is dissolved in 3 ml of dioxane
7. 7
   workup.ADDITIONtreated with 4 N HCl in dioxane

Vorschrift

0.2 g (0.6 mmol) of 2-chloro-9-ethyl-6-(3-cyano-phenyl-amino)-9H-purine is stirred in 2.5 ml of ethylenediamine at 75° C. for 3.5 h, and the mixture is allowed to cool and is diluted with ethyl acetate. The organic phase is washed with water, separated off and dried over sodium sulfate. After removal of the solvent, the residue is dissolved in 3 ml of dioxane and treated with 4 N HCl in dioxane. 2-(2-Amino-ethyl-amino)-6-(3-cyano-phenyl-amino)-9-ethyl-9H-purine hydrochloride is obtained as a crystalline precipitate. This is filtered off and dried; m.p. 200° C.; FAB-MS: (M+H)+=323; Rf=0.5 (ethyl acetate:i-propanol:water: 22% aqueous ammonium hydroxide solution=40:60:15:10).

Quelle