反应详情

To a stirred solution of 8-chloro-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (0.20, 0.67 mmol) in THF (5 ml) was added 3-[5-(phenylmethyl)-1,2,4-oxadiazol-3-yl]-1-propanol (0.162 g, 0.74 mmol), DBAD (0.186 g, 0.81 mmol) and triphenylphosphine (0.212 g, 0.81 mmol) and the solution stirred for 18 h. To the solution was added Pd(PPh3)4 (75 mg, 0.067 mmol) and morpholine (604 μl, 6.7 mmol) were added and stirred for at rt under nitrogen for a further 3 h. 75 mg of Pd(PPh3)4 was added and the mixture left to stir for another 3 h. The mixture was partitioned between EtOAc and 2M HCl (aq). The organic layer was separated, washed with brine, dried (MgSO4) and concentrated. The crude material was purified by an aminopropyl SPE using MeOH to load the compound onto the column and wash through the impurities, then with 2-4% AcOH/MeOH to elute the compound. The product fractions were combined and concentrated then further purified by MDAP. The product fractions were combined and concentrated give the title compound as a white solid (51 mg, 20%).

1. additionwere added
2. stirringstirred for at rt under nitrogen for a further 3 h
3. waitthe mixture left
4. stirringto stir for another 3 h
5. customThe mixture was partitioned between EtOAc and 2M HCl (aq)
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated
10. customThe crude material was purified by an aminopropyl SPE
11. washwash through the impurities
12. washwith 2-4% AcOH/MeOH to elute the compound
13. concentrationconcentrated
14. customthen further purified by MDAP
15. concentrationconcentrated