Реакция #10010

Уравнение реакции

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

Растворители

ethylenediamine

ethyl acetate

Условия реакции

Обработка

1. 1
   Температураto cool
2. 2
   ПромывкаThe organic phase is washed with water
3. 3
   Другоеseparated off
4. 4
   Сушкаdried over sodium sulfate
5. 5
   ДругоеAfter 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

Методика

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).

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