反应详情

温度

45 °C

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 DMF (2 ml) was stirred with sodium carbonate (64 mg, 0.6 mmol) and 2-chloro-6-fluorobenzyl bromide (134 mg, 0.6 mmol) and heated at 45° C. for 18 h under nitrogen. After cooling to rt the mixture was degassed by evacuating and readmitting nitrogen, and stirred with tetrakis(triphenylphosphine)palladium(0) (35 mg, 0.303 mmol) and morpholine (0.13 ml) for 5.5 h. The mixture was partitioned between EtOAc and 2M HCl, the organic phase separated and evaporated and the residue purified by aminopropyl SPE (5 g, washing with THF-MeOH (1:1) then neat MeOH and finally eluting with DCM-MeOH (1:1) containing 5% AcOH) to give the title compound (57 mg) as a solid.

1. temperatureAfter cooling to rt the mixture
2. customwas degassed
3. customby evacuating
4. customThe mixture was partitioned between EtOAc and 2M HCl
5. customthe organic phase separated
6. customevaporated
7. customthe residue purified by aminopropyl SPE (5 g
8. washwashing with THF-MeOH (1:1)
9. washneat MeOH and finally eluting with DCM-MeOH (1:1)
10. additioncontaining 5% AcOH)