反应详情

温度

60 °C

A stirring mixture of N2-butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (3.25 gm) and potassium carbonate (3.83 gm) in dry N,N-dimethylformamide (30 ml) was heated with stirring at 60° C. for 1 h. Tetrahydro-3-furanylmethyl methanesulfonate (2 gm, Isomer 1) was added and the stirring mixture heated at 90° C. for 3 h. The solvent was evaporated, water was added and the mixture extracted three times with ethyl acetate. The combined extracts were washed with water then brine, dried by passing through a hydrophobic frit and stripped to give an orange solid. This was purified by C18 reverse phase chromatography using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluent (20-60%) and the appropriate fractions combined and evaporated to give the title compound as a light orange solid, yield 1.56 gm.

1. temperaturewas heated
2. temperaturethe stirring mixture heated at 90° C. for 3 h
3. customThe solvent was evaporated
4. additionwater was added
5. extractionthe mixture extracted three times with ethyl acetate
6. washThe combined extracts were washed with water
7. dry with materialbrine, dried
8. customto give an orange solid
9. customThis was purified by C18 reverse phase chromatography
10. customevaporated