反应详情

温度

60 °C

To a solution of 2-[(2-cyclopropylethyl)oxy]-8-(methoxy)-1H-purin-6-amine trifluoroacetic acid salt (2.89 g) in dry N,N-dimethylformamide (32 ml) under nitrogen and at room temperature, was added potassium carbonate (4.41 g) in one go. The reaction was heated to 60° C. and stirred for 90 minutes. A solution of tetrahydro-3-furanylmethyl methanesulfonate, Isomer 2 (1.869 g) in dry DMF (3 ml) was then added gradually via pipette. The reaction was heated to 70° C. and left to stir overnight. Still 22% starting material present by LCMS, therefore increased temperature to 90° C. and stirred for a further 3 hours at this temperature. The reaction was cooled and diluted with ethyl acetate (100 ml) and washed with water (50 ml) and brine (50 ml). The organic layer was concentrated in vacuo to yield an orange oil. The product was purified by C18 reverse phase chromatography using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluant (10-60%) to afford the title compound as an orange viscous oil (1.45 g).

1. temperatureThe reaction was heated to 70° C.
2. waitleft
3. stirringto stir overnight
4. temperatureincreased temperature to 90° C.
5. stirringstirred for a further 3 hours at this temperature
6. temperatureThe reaction was cooled
7. washwashed with water (50 ml) and brine (50 ml)
8. concentrationThe organic layer was concentrated in vacuo
9. customto yield an orange oil
10. customThe product was purified by C18 reverse phase chromatography