反应 #10015

反应方程式

2-chloro-6-(4-nitro-phenyl-amino)-purine

caesium carbonate

isopropyl iodide

dioxane

→

2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine

溶剂

ethyl acetate

—

mixture

DMF

water

反应条件

后处理

1. 1
   洗涤the organic phase is washed with water
2. 2
   干燥dried over sodium sulfate
3. 3
   其他After removal of the solvent
4. 4
   其他the residue is chromatographed over silica gel (mobile phase: CH2Cl2:methanol=9:1)
5. 5
   其他The crystalline precipitate obtained on concentration
6. 6
   过滤is filtered off
7. 7
   其他dried

实验过程

A mixture comprising 0.87 g (3 mmol) of 2-chloro-6-(4-nitro-phenyl-amino)-purine, 0.15 g (4.5 mmol) of caesium carbonate and 1.8 ml (18 mmol) of isopropyl iodide is stirred in 22 ml of a mixture comprising dioxane:water:DMF in a ratio of 2:1:4 at 100° C. for 48 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is chromatographed over silica gel (mobile phase: CH2Cl2:methanol=9:1). The crystalline precipitate obtained on concentration is filtered off and dried. 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine is obtained; m.p.>260° C.; FAB-MS: (M+H)+=333; Rf=0.8 (CH2Cl2:methanol=9:1).

来源