反应详情

N2-Butyl-8-(methoxy)-3H-purine-2,6-diamine trifluoroacetic acid salt (0.25 g) and anhydrous potassium carbonate (0.395 g) in anhydrous DMF (3 mL) was heated for 1 hour at 60° C. (external) under nitrogen, before being allowed to cool to room temperature. To the reaction mixture was then added 3-(bromomethyl) tetrahydrofuran (0.236 g) and the reaction mixture heated under nitrogen to 50° C. (external) for 18.5 hours. The reaction mixture was then diluted with water (15 mL) and extracted with diethyl ether (15 mL, 3 times). The organic layers were combined and dried over anhydrous sodium sulphate. The sodium sulphate was filtered off and the filtrate evaporated under reduced pressure to give an oil. This oil was triturated with cyclohexane and a little diethyl ether to give a solid. The cyclohexane and diethyl ether was evaporated under reduced pressure to give a white solid. The solid (0.2606 g) was dissolved in hot ethanol (2 mL). To this solution was then added water (8 mL) and the resultant suspension was heated to reflux (93° C., external) giving a solution. The solution was then allowed to cool slowly (by not removing the flask from the reaction block and turning the power off to the heating block). This gave a solid gum on cooling which when sonicated gave a white solid. This solid was isolated by filtration under suction and then dried under vacuo at 50° C., overnight. This gave the title compound (0.1043 g) as a white solid.

1. extractionextracted with diethyl ether (15 mL, 3 times)
2. dry with materialdried over anhydrous sodium sulphate
3. filtrationThe sodium sulphate was filtered off
4. customthe filtrate evaporated under reduced pressure
5. customto give an oil
6. customThis oil was triturated with cyclohexane
7. customa little diethyl ether to give a solid
8. customThe cyclohexane and diethyl ether was evaporated under reduced pressure
9. customto give a white solid
10. temperatureto reflux (93° C., external)
11. customgiving a solution
12. temperatureto cool slowly (by not
13. customremoving the flask from the reaction block
14. customThis gave a solid gum
15. temperatureon cooling which when
16. customsonicated
17. customgave a white solid
18. customThis solid was isolated by filtration under suction
19. customdried under vacuo at 50° C., overnight