反应详情

To a suspension of 7.1 g (0.021 mole) of 9-benzyl-2,3-dihydro-1,3-dimethyl-6-hydroxy-pyrimido[2,1-f]purine-4,8(1H,9H)-dione in 200 ml of acetone, add 2.3 g (0.023 mole) of triethylamine, and stir the mixture for 5 minutes at room temperature under a nitrogen atmosphere to obtain a clear solution. Add dropwise to the solution 4.7 g (0.027 mole) of benzyl bromide, and reflux the mixture for 5 hours under a nitrogen atmosphere. Remove the acetone under reduced pressure, and triturate the gummy residue with methanol. Filter off the resultant white solid, pour the filtrate into water, acidify to pH 4-5 with dilute hydrochloric acid, and decant the aqueous supernatant. Dissolve the gummy residue in the chloroform, wash the solution with water, and dry over anhydrous magnesium sulfate. Remove the drying agent by filtration, and evaporate solvent from the filtrate under reduced pressure. Chromatograph the residual oil on silica gel, eluting with chloroform(96)-methanol(4), to obtain the title compound as a solid with mp 176°-179° C.

1. customto obtain a clear solution
2. temperaturereflux the mixture for 5 hours under a nitrogen atmosphere
3. customRemove the acetone under reduced pressure
4. customtriturate the gummy residue with methanol
5. filtrationFilter off the resultant white solid
6. additionpour the filtrate into water
7. customdecant the aqueous supernatant
8. dissolutionDissolve the gummy residue in the chloroform
9. washwash the solution with water
10. dry with materialdry over anhydrous magnesium sulfate
11. customRemove the drying agent
12. filtrationby filtration
13. customevaporate solvent from the filtrate under reduced pressure
14. washChromatograph the residual oil on silica gel, eluting with chloroform(96)-methanol(4)