反应详情

To 8-chloro-3-pentyl-7-(2-propen-1-yl)-1-[3-(1H-pyrazol-4-yl)propyl]-3,7-dihydro-1H-purine-2,6-dione (61 mg, 0.15 mmol) in dry THF (1 ml) at −78° C., under nitrogen, was added potassium t-butoxide (1M in THF, 0.15 ml), followed by 2-chloro-5-(chloromethyl)thiophene (25 mg, 0.15 mmol). Stirring was continued at −78° C. for 15 min, then at room temperature for 1 h and finally at 60° C. for 18 h. The solution was degassed and morpholine (0.13 ml) and tetrakis(triphenylphosphine)palladium(0) (35 mg) added and stirring continued for 6 h. Further quantities (0.2 ml morpholine, 50 mg Pd(PPh3)4) were added and stirring continued overnight. Worked up by partition between EtOAc and 2M HCl, the organic phase evaporated and purified by the standard aminopropyl SPE procedure followed by MDAP yielding title compound as a white solid (5.1 mg).

1. waitat room temperature for 1 h
2. waitfinally at 60° C. for 18 h
3. customThe solution was degassed
4. additionmorpholine (0.13 ml) and tetrakis(triphenylphosphine)palladium(0) (35 mg) added
5. stirringstirring
6. waitcontinued for 6 h
7. additionFurther quantities (0.2 ml morpholine, 50 mg Pd(PPh3)4) were added
8. stirringstirring continued overnight
9. customby partition between EtOAc and 2M HCl
10. customthe organic phase evaporated
11. custompurified by the standard aminopropyl SPE procedure