反应详情

温度

60 °C

To a solution of 2-[(2-Cyclopropylethyl)oxy]-8-methoxy-9H-purin-6-amine trifluoroacetic acid salt (300 mg) in dry DMF (5 mL) was added anhydrous potassium carbonate (457 mg) and the mixture was heated at 60° C. for 1.5 h. The reaction was cooled to room temperature and tetrahydro-3-furanylmethyl methanesulfonate (164 mg) was added. The reaction was heated at 90° C. for 3.5 h and was then quenched into water (50 mL) and extracted with EtOAc (3×50 mL). The organics were separated, dried by passing through a hydrophobic frit and evaporated under reduced pressure to give a glassy solid. The material was purified by C18 reverse phase chromatography (ISCO) using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluent (20-60%) to give the title compound (103.8 mg).

1. temperatureThe reaction was cooled to room temperature
2. temperatureThe reaction was heated at 90° C. for 3.5 h
3. customwas then quenched into water (50 mL)
4. extractionextracted with EtOAc (3×50 mL)
5. customThe organics were separated
6. customdried
7. customevaporated under reduced pressure
8. customto give a glassy solid
9. customThe material was purified by C18 reverse phase chromatography (ISCO)