反应 #10013

反应方程式

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

caesium carbonate

isopropyl iodide

dioxane

→

2-chloro-9-isopropyl-6-(4-fluoro-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After drying over sodium sulfate and removal of the solvent
3. 3
   其他the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1)
4. 4
   浓缩On concentration

实验过程

A mixture comprising 1 g (3.3 mmol) of 2-chloro-6-(4-fluoro-phenyl-amino)-purine, 2.1 g (6.6 mmol) of caesium carbonate and 2 ml of isopropyl iodide is stirred in 32 ml of a mixture comprising dioxane, water and DMF in a ratio of 2:3:7 at 100° C. for 20 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water. After drying over sodium sulfate and removal of the solvent, the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1). On concentration, 2-chloro-9-isopropyl-6-(4-fluoro-phenyl-amino)-9H-purine is obtained as a crystalline compound. m.p. 154° C.; FAB-MS: (M+H)+=306; Rf=0.2 (ethyl acetate:hexane=4:1).

来源