反应详情

温度

60 °C

To a 0.27 M solution of hydroxyl-quinolinone from Step 3 (1 eq.) and brosylate from Step 2 (1 eq.) in N-methyl-2-pyrrolidinone was added cesium carbonate (1.5 eq.) and the resulting mixture was heated at 60° C. for 16 h. The mixture was cooled to RT and partitioned between water and EtOAc. The organic phase was washed with brine, dried (Na2SO4) and the volatiles were removed under reduced pressure. The residue was purified by SiO2 gel chromatography (eluting with 50% EtOAc/Hex and then 0-5% MeOH/DCM) to yield the title compound. MS (ES+) C29H38BrN3O8 requires: 637. Found: 636, 638 (M+H+).

1. temperatureThe mixture was cooled to RT
2. custompartitioned between water and EtOAc
3. washThe organic phase was washed with brine
4. dry with materialdried (Na2SO4)
5. customthe volatiles were removed under reduced pressure
6. customThe residue was purified by SiO2 gel chromatography (
7. washeluting with 50% EtOAc/Hex