反应详情

温度

100 °C

To a heterogeneous mixture of 2-(bromomethyl)-5-chloro-3-(2-chloro-5-fluoro-phenyl)quinoxaline (0.1815 g, 0.4702 mmol) in DMF (3.444 mL, 0.4702 mmol) was added potassium phthalimide (0.2177 g, 1.175 mmol) and the heterogeneous mixture was stirred at 100° C. After stirring at 100° C. for 30 min, the mixture was concentrated under reduced pressure and triturated with water (30 mL). The precipitate was collected by filtration. The resulting solid was filtered and washed with 2 N NaOH (30 mL) and then with water (100 mL), and air-dried to give 2-((5-chloro-3-(2-chloro-5-fluorophenyl)quinoxalin-2-yl)methyl)isoindoline-1,3-dione as an off-white solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 8.09 (1H, dd, J=7.6, 1.4 Hz), 7.95-8.01 (1H, m), 7.82-7.91 (5H, m), 7.65-7.75 (2H, m), 7.43-7.52 (1H, m), 4.99 (2H, br. s.); LC-MS (ESI) m/z 452.0 [M+H]+. The crude product was carried on crude without purification for the next step.

1. stirringAfter stirring at 100° C. for 30 min
2. concentrationthe mixture was concentrated under reduced pressure
3. customtriturated with water (30 mL)
4. filtrationThe precipitate was collected by filtration
5. filtrationThe resulting solid was filtered
6. washwashed with 2 N NaOH (30 mL)
7. dry with materialwith water (100 mL), and air-dried