반응 #10013

반응 방정식

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

caesium carbonate

isopropyl iodide

dioxane

→

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

용매

ethyl acetate

—

mixture

DMF

water

반응 조건

후처리

1. 1
   세척the organic phase is washed with water
2. 2
   건조After drying over sodium sulfate and removal of the solvent
3. 3
   기타the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1)
4. 4
   농축On concentration

실험 절차

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).

출처