反应详情

3-Benzoyl-1-(4-chloro-butyl)-5-iodo-1H-pyrimidine-2,4-dione (Prep 44, 433 mg, 1 mmol) was dissolved in degassed DME-water solution (5-1, 30 mL). 2-methyl-pyridine 4-boronic acid (205 mg, 1.5 mmol), Na2CO3 (212 mg, 2 mmol), 2-(dicyclohexylphosphino)biphenyl (70 mg, 0.2 mmol) and Pd(PPh3)4 (231 mg, 0.2 mmol) were added and the mixture was refluxed for 6 hours. The solvents were evaporated under vacuum and the crude was partitioned between ethyl acetate and water. The organic phase was dried (Na2SO4) and evaporated; the crude was purified by flash chromatography with DCM-MeOH—NH4OH (98-2-0.2) and SCX cartridge washing with MeOH and eluting with MeOH/NH3 95:5 to give the title compound (100 mg, 25% yield).

1. temperaturethe mixture was refluxed for 6 hours
2. customThe solvents were evaporated under vacuum
3. customthe crude was partitioned between ethyl acetate and water
4. dry with materialThe organic phase was dried (Na2SO4)
5. customevaporated
6. customthe crude was purified by flash chromatography with DCM-MeOH—NH4OH (98-2-0.2) and SCX cartridge
7. washwashing with MeOH
8. washeluting with MeOH/NH3 95:5