反応 #10013

反応方程式

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

caesium carbonate

isopropyl iodide

dioxane

→

2-chloro-9-isopropyl-6-(4-fluoro-phenyl-amino)-9H-purine

溶媒

ethyl acetate

—

mixture

DMF

water

反応条件

後処理

1. 1
   洗浄the organic phase is washed with water
2. 2
   乾燥After drying over sodium sulfate and removal of the solvent
3. 3
   その他the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1)
4. 4
   濃縮On concentration

実験手順

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).

出典