反应 #10005

反应方程式

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

→

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

溶剂

ethylenediamine

ethyl acetate

反应条件

后处理

1. 1
   温度to cool
2. 2
   洗涤The organic phase is washed with water
3. 3
   其他separated off
4. 4
   干燥dried over sodium sulfate
5. 5
   其他After removal of the solvent
6. 6
   workup.DISSOLUTIONthe residue is dissolved in dioxane
7. 7
   workup.ADDITIONtreated with 4 N HCl in dioxane

实验过程

0.2 g (0.62 mmol) of 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine is stirred in 2.5 ml of ethylenediamine at 75° C. for 3 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 dioxane, and treated with 4 N HCl in dioxane. 2-(2-Amino-ethyl-amino)-9-ethyl-6-(3-fluor-phenyl-amino)-9H-purine hydrochloride is obtained as a crystalline precipitate by this procedure. This precipitate is filtered off and dried; m.p.>250° C.; FAB-MS: (M+H)+=315; Rf=0.6 (ethyl acetate:isopropanol:water:22% aqueous ammonium hydroxide solution=40:60:15:18).

来源