反应详情

温度

60 °C

To a solution of N2-butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (100 mg) in dry N,N-dimethylformamide (1 ml) at room temperature and under nitrogen was added potassium carbonate (158 mg) in one go. The reaction was stirred at 60° C. for 1.5 hours and then cooled to 50° C. A solution of 3-(bromomethyl)tetrahydro-2H-pyran (56 mg) in dry N,N-dimethylformamide (0.3 ml) was added in one go and the reaction heated at 50° C. for 16 hours. The reaction was diluted with ethyl acetate (15 ml) and washed with water (5 ml). The organic layer was separated, dried over magnesium sulphate, filtered, and concentrated in vacuo. The product was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (20-60%) to afford the title compound as a yellow oil (45 mg).

1. temperaturecooled to 50° C
2. temperaturethe reaction heated at 50° C. for 16 hours
3. washwashed with water (5 ml)
4. customThe organic layer was separated
5. dry with materialdried over magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe product was purified by C18 reverse phase chromatography