反应详情

温度

60 °C

To a solution of N2-butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (500 mg) in dry N,N-dimethylformamide (8 ml) at room temperature and under nitrogen was added potassium carbonate (1.17 g) in one go. The reaction was stirred at 60° C. for 1.5 hours and then cooled to room temperature. 4-(bromomethyl)tetrahydro-2H-pyran (0.3 ml) was added in one go and the reaction heated at 50° C. overnight. The reaction was diluted with ethyl acetate (20 ml) and washed with water (10 ml). The organic layer was separated 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 (10-45%) to afford the title compound as a yellow viscous oil (315 mg, 90% clean).

1. temperaturecooled to room temperature
2. temperaturethe reaction heated at 50° C. overnight
3. washwashed with water (10 ml)
4. customThe organic layer was separated
5. concentrationconcentrated in vacuo
6. customThe product was purified by C18 reverse phase chromatography