反応 #10010

反応方程式

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

溶媒

ethylenediamine

ethyl acetate

反応条件

後処理

1. 1
   温度to cool
2. 2
   洗浄The organic phase is washed with water
3. 3
   その他separated off
4. 4
   乾燥dried over sodium sulfate
5. 5
   その他After 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

実験手順

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).

出典