反应详情

温度

60 °C

To a solution of N2-(2-cyclopropylethyl)-8-(methoxy)-9H-purine-2,6-diamine trifluoroacetate (400 mg) in N,N-dimethylformamide (6.90 ml) at room temperature was added potassium carbonate (610 mg) and the reaction stirred at 60° C. for 90 minutes. The reaction mixture was cooled to room temperature and tetrahydro-2H-pyran-3-ylmethyl methanesulfonate (236 mg) was added. Stirring was continued at 50° C. for 20 hours. The reaction temperature was increased to 90° C. and stirring continued. The reaction was cooled and taken up in ethyl acetate (50 ml) and washed with water (2×50 ml). The organic layer was separated, dried over magnesium sulfate, filtered and concentrated in vacuo to give an orange oil. The product was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (10-50%) to afford the title compound as a colourless oil (198 mg, 88% pure).

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringStirring
3. waitwas continued at 50° C. for 20 hours
4. temperatureThe reaction temperature was increased to 90° C.
5. stirringstirring
6. temperatureThe reaction was cooled
7. washwashed with water (2×50 ml)
8. customThe organic layer was separated
9. dry with materialdried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated in vacuo
12. customto give an orange oil
13. customThe product was purified by C18 reverse phase chromatography