反应详情

A mixture comprising 1 g (3.2 mmol) of 2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine, 1.7 g (5.1 mmol) of caesium carbonate and 2.1 ml (25.6 mmol) of ethyl iodide in 7 ml of dioxane/water/DMF (8:2:2) is stirred at RT for 18 h. It is then diluted with ethyl acetate and the organic phase is washed with water. This phase is separated off and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 129–130° C.; FAB-MS: (M+H)+=342; Rf=0.6 (methylene chloride:methanol=9:1).

1. washthe organic phase is washed with water
2. customThis phase is separated off
3. dry with materialdried over sodium sulfate
4. customAfter removal of the solvent
5. customthe residue is recrystallized from ethyl acetate and diethyl ether