反应详情

温度

65 °C

A mixture of 3-bromo-7-trifluoromethylimidazo[1,2-a]pyrimidine (139 mg, 0.53 mmol), the foregoing boronate ester (269 mg, 1.05 mmol) and K3PO4 (483 mg, 2.1 mmol) in DMA (3 ml) was degassed with a stream of N2 for 5 min and then tetrakis(triphenylphosphine)palladium(0) (60 mg, 10 mol %) was added and the reaction heated at 65° C. for 70 min. EtOAc (100 ml) was added and the mixture washed with H2O (3×100 ml) and brine (100 ml), dried (MgSO4) and concentrated under reduced pressure while dry loading onto silica. The residue was purified by column chromatography on silica using 5% MeOH in dichloromethane to yield 3-[3-([1,2,4]triazol-4-yl)phenyl]-7-trifluoromethylimidazo[1,2-a]pyrimidine (70 mg, 40%), which was then recrystallised from EtOAc/isohexanes: δH (400 MHz, d6-DMSO) 7.55 (1H, d, J 7.2), 7.70-7.90 (3H, m), 8.16 (1H, s), 8.39 (1H, s), 9.24 (2H, s), 9.48 (1H, d, J 7.2); m/z (ES+) 331 (M+H+).

1. washthe mixture washed with H2O (3×100 ml) and brine (100 ml)
2. dry with materialdried (MgSO4)
3. concentrationconcentrated under reduced pressure
4. customwhile dry loading onto silica
5. customThe residue was purified by column chromatography on silica using 5% MeOH in dichloromethane