反应详情

3-Benzoyl-1-(3-chloro-propyl)-5-iodo-1H-pyrimidine-2,4-dione (Prep 41,500 mg, 1.2 mmol) was dissolved in degassed DME-water solution (5-1, 35 mL). Pyridine-3-boronic acid (629 mg, 1.8 mmol), Na2CO3 (380 mg, 3.6 mmol), 2-(dicyclohexylphosphino)biphenyl (84 mg, 0.24 mmol) and Pd(PPh3)4 (250 mg, 0.24 mmol) were added and the mixture was refluxed for 3 hours. The solvents were evaporated under vacuum and the residue was filtered over a SCX cartridge washing with MeOH and eluting with MeOH/NH3 95:5. The crude was purified by flash chromatography with DCM-MeOH—NH4OH (from 98-2-0.2 to 95:5:05) to give the title compound (90 mg, 20% yield).

1. temperaturethe mixture was refluxed for 3 hours
2. customThe solvents were evaporated under vacuum
3. filtrationthe residue was filtered over a SCX cartridge
4. washwashing with MeOH
5. washeluting with MeOH/NH3 95:5
6. customThe crude was purified by flash chromatography with DCM-MeOH—NH4OH (from 98-2-0.2 to 95:5:05)