Reacción #10013

Ecuación de reacción

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

caesium carbonate

isopropyl iodide

dioxane

→

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

Disolventes

ethyl acetate

—

mixture

DMF

water

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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).

Fuente