Реакция #10013

Уравнение реакции

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

caesium carbonate

isopropyl iodide

dioxane

→

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

Растворители

ethyl acetate

—

mixture

DMF

water

Условия реакции

Обработка

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

Методика

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).

Источник