反应详情

温度

150 °C

To a solution of [(3-bromo-4-fluorophenyl)methyl]methylamine (0.52 g, 2.39 mmol) in p-dioxane/H2O (15/5 mL) was added {3-[(4-{[(1,1-dimethylethyl)oxy]carbonyl}-1-piperazinyl)methyl]phenyl}boronic acid (1.15 g, 3.60 mmol), Pd(PPh3)4 (139 mg, 0.12 mmol), and K2CO3 (1.33 g, 9.6 mmol). The mixture was heated with a microwave at 150° C. for 15 min. The organic layer was separated, concentrated. The residue was redissolved in EtOAc (˜70 mL), which was washed with H2O (20 mL), brine (20 mL), dried over Na2SO4, filtered, concentrated and purified by CombiFlash chromatograph to afford the title compound 0.65 g (66%). LC-MS m/z 414 (M+H)+.

1. customThe organic layer was separated
2. concentrationconcentrated
3. dissolutionThe residue was redissolved in EtOAc (˜70 mL)
4. washwhich was washed with H2O (20 mL), brine (20 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified by CombiFlash chromatograph