反应详情

温度

50 °C

Cs2CO3 (10.7 g, 32.9 mmol) was added to a stirred mixture of 1-tert-butyl 2-methyl (2S,4S)-4-{[(4-bromophenyl)sulfonyl]oxy}pyrrolidine-1,2-dicarboxylate (8.78 g, 18.9 mmol) and 2-bromo-6-methoxyquinolin-3-ol (4.18 g, 16.45 mmol) in NMP (46 mL). The resulting mixture was stirred at 50° C. for 3 h, then cooled and diluted with EtOAc. The organics were washed with saturated aqueous NaHCO3, water and brine then dried over Na2SO4. Filtration and removal of the volatiles gave a residue, which was purified by column chromatography on silica gel (gradient elution: 1 to 100% EtOAc in petroleum ether) to give the title compound (5.56 g, 70.2%). LCMS (ES+) m/z 481, 483 (M+H)+.

1. temperaturecooled
2. washThe organics were washed with saturated aqueous NaHCO3, water and brine
3. dry with materialthen dried over Na2SO4
4. filtrationFiltration and removal of the volatiles
5. customgave a residue, which
6. customwas purified by column chromatography on silica gel (gradient elution: 1 to 100% EtOAc in petroleum ether)