反应详情

A mixture of N2-butyl-9-(3-chloropropyl)-8-(methyloxy)-9H-purine-2,6-diamine (250 mg, 0.8 mmole), piperidine (340 mg, 4 mmole) and sodium iodide (360 mg, 2,4 mmole) in THF (8 ml) was heated under reflux for 48 hours. The solvent was evaporated and the residue purified by preparative TLC then dissolved in methanol (5 ml). Hydrogen chloride in methanol (0.5 ml) was added and the mixture stirred at room temperature for 16 hours. The solvent was then evaporated and the pH of the residue was adjusted to 7-8 by addition of sodium bicarbonate solution. The product was extracted into ethyl acetate and the extract was evaporated and the residue purified by preparative HPLC to give the title compound (16 mg).

1. temperaturewas heated
2. temperatureunder reflux for 48 hours
3. customThe solvent was evaporated
4. customthe residue purified by preparative TLC
5. dissolutionthen dissolved in methanol (5 ml)
6. additionHydrogen chloride in methanol (0.5 ml) was added
7. customThe solvent was then evaporated
8. additionthe pH of the residue was adjusted to 7-8 by addition of sodium bicarbonate solution
9. extractionThe product was extracted into ethyl acetate
10. customthe extract was evaporated
11. customthe residue purified by preparative HPLC