反应详情

温度

60 °C

A stirring mixture of 2-[(2-cyclopropylethyl)oxy]-8-(methoxy)-1H-purin-6-amine trifluoroacetic acid salt (2.89 g), potassium carbonate (4.41 g) and dry DMF (32 ml) was heated at 60° C. under nitrogen for 90 minutes. Tetrahydro-3-furanylmethyl methanesulfonate (1.869 g, isomer 1) was then added and stirring continued at 70° C. for 1 h, then at 90° C. for 2 h. The solvent was evaporated and the residue treated with water and extracted three times with ethyl acetate. The combined extracts were washed with water then brine, dried by passing through a hydrophobic frit and evaporated to a brown oil. This was purified on a 360 gm C18 column using water (+0.1% formic acid)/acetonitrile (+0.05% formic acid). Appropriate fractions were combined and evaporated, yield 814 mg.

1. waitat 90° C. for 2 h
2. customThe solvent was evaporated
3. additionthe residue treated with water
4. extractionextracted three times with ethyl acetate
5. washThe combined extracts were washed with water
6. dry with materialbrine, dried
7. customevaporated to a brown oil
8. customThis was purified on a 360 gm C18 column
9. customevaporated