反应详情

温度

110 °C

A mixture of 6-t-Butoxycarbonyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-ylamine, Intermediate 3 (500 mg, 2.0 mmol), 5-bromo-1,2,3-trimethoxybenzene (494 mg, 2.0 mmol), Cl-BrettPhos-Pd precatalyst/BrettPhos admixture (53 mg, 0.040 mmol (1:1 mol: mol)) and cesium carbonate (912 mg, 2.80 mmol) in t-BuOH (15 mL) was heated at 110° C. for 16 hours. Upon cooling, the reaction mixture was diluted with EtOAc and the insolubles were filtered off (celite). The filtrate was concentrated and the residue was eluted through a flash column (silica gel 60, 230-400 mesh, 2:3 hexanes:EtOAc) to obtain a clear glass (659 mg, 79%).

1. temperatureUpon cooling
2. filtrationthe insolubles were filtered off (celite)
3. concentrationThe filtrate was concentrated
4. washthe residue was eluted through a flash column (silica gel 60, 230-400 mesh, 2:3 hexanes:EtOAc)