反应详情

温度

0 °C

To a mixture of (R)—N-(3-fluoro-4-(7-methoxyquinolin-4-yloxy)-phenyl-1-(2-hydrox-ylpropyl)-5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide (1.08 g, 2.0 mmol), N,N-dimethylglycine (0.516 g, 5 mmol Alfa Aesar), HATU (1.902 g. 5 mmol) and DMAP (62.5 mg, 0.5 mmol, Aladdin) was added TEA (1.012 g, 10 mmol) in DMF (12.5 mL) under nitrogen atmosphere at 0° C. The reaction was stirred at 0° C. for 2 hrs, and then warmed up to room temperature and continued to stir overnight. The reaction was diluted with 100 mL of CH2Cl2. The resulted solution was washed with 0.1 N HCl (10 mL×2), saturated NaHCO3 (20 mL×2) and followed by water (20 mL). The organic phase was dried over Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc/MeOH=2/1) to give the title compound as a yellow solid (1.1367 g, 84%).

1. temperaturewarmed up to room temperature
2. stirringto stir overnight
3. washThe resulted solution was washed with 0.1 N HCl (10 mL×2), saturated NaHCO3 (20 mL×2)
4. dry with materialThe organic phase was dried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by a silica gel column chromatography (EtOAc/MeOH=2/1)