反应详情

温度

60 °C

8-(Methoxy)-2-{[2-(methoxy)ethyl]oxy}-9H-purin-6-amine trifluoroacetate salt (0.30 g) was dissolved in dry DMF (5 mL). To this was added anhydrous potassium carbonate (0.47 g) and then heated to 60° C. for 1.5 hours. The reaction mixture was cooled to room temperature and tetrahydro-3-furanylmethyl methanesulfonate (0.168 g) was added. The reaction mixture was then heated to 90° C. for 3.5 hours. The reaction mixture was then quenched into water (100 mL) and extracted into ethyl acetate (50 mL, 3 times). The organic was separated and dried by passing through a hydrophobic frit and then evaporated under reduced pressure to give a glassy solid. This was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluent (10-45%). This gave the title compound as a white solid (0.1233 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. temperatureThe reaction mixture was then heated to 90° C. for 3.5 hours
3. customThe reaction mixture was then quenched into water (100 mL)
4. extractionextracted into ethyl acetate (50 mL, 3 times)
5. customThe organic was separated
6. customdried
7. customevaporated under reduced pressure
8. customto give a glassy solid
9. customThis was purified by C18 reverse phase chromatography