反应详情

温度

40 °C

Cs2CO3 (1.1 g, 3.39 mmol) was added to a solution of 2-but-3-en-1-ylisoquinoline-1,3(2H,4H)-dione (0.49 g, 2.26 mmol) and 1-t-butyl 2-methyl (2S,4S)-4-{[(4-bromophenyl)sulfonyl]oxy}pyrrolidine-1,2-dicarboxylate (1.05 g, 2.26 mmol) in NMP (10 mL), and the reaction mixture was stirred for 16 hours at 40° C. An additional portion of 1-t-butyl 2-methyl (2S,4S)-4-{[(4-bromophenyl)sulfonyl]oxy}pyrrolidine-1,2-dicarboxylate (1.0 g, 2.16 mmol) was added, and the reaction mixture was stirred at 40° C. for 16 hours. The reaction mixture was cooled and poured onto a mixture of EtOAc and H2O, and the layers were separated. The organic layer was washed with H2O (2×), 1N HCl (1×) and brine, dried over Na2SO4, filtered and concentrated in vacuo. The resulting residue was purified by column chromatography (gradient elution, 10-40% EtOAc/Hexane) to afford the title compound (0.83 g, 83%) as an oil. LCMS (ES+) m/z 443.0 (M+H)+.

1. stirringthe reaction mixture was stirred at 40° C. for 16 hours
2. temperatureThe reaction mixture was cooled
3. customthe layers were separated
4. washThe organic layer was washed with H2O (2×), 1N HCl (1×) and brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe resulting residue was purified by column chromatography (gradient elution, 10-40% EtOAc/Hexane)