反应详情

温度

80 °C

To a 250-mL RB flask containing tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3,6-dihydro-1(2H)-pyridinecarboxylate (3.31 g, 10.7 mmol), K2CO3 (4.44 g, 32.1 mmol) and PdCl2dppf (870 mg, 1.07 mmol) was added a solution of N-(5-bromo-2,4-difluorophenyl)-2-methylpropanamide (3.28 g, 11.8 mmol) in DMF (100 mL) at room temperature under argon. The mixture was heated to 80° C. under argon overnight, cooled to room temperature, filtered through celite and the celite was washed with EtOAc (3×20 mL). The filtrates were washed with H2O (20 mL), brine (20 mL), dried over MgSO4, filtered and concentrated in vacuo. The crude material was purified by flash chromatography (10%–20% EtOAc/hexane) to give 2.4 g (6.31 mmol, 59%) of tert-butyl 4-[2,4-difluoro-5-(isobutyrylamino)phenyl]-3,6-dihydro-1(2H)-pyridine carboxylate: ESMS m/e: 379.3 (M−H)+.

1. temperaturecooled to room temperature
2. filtrationfiltered through celite
3. washthe celite was washed with EtOAc (3×20 mL)
4. washThe filtrates were washed with H2O (20 mL), brine (20 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude material was purified by flash chromatography (10%–20% EtOAc/hexane)