反应详情

温度

100 °C

Under nitrogen atmosphere, to the N,N-dimethyl formamide (1.5 ml) solution of 9-bromo-8-(4-cyclobutyl-piperazin-1-yl)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound F4-10, 50 mg, 0.099 mmol), trimethyl boroxine (12 mg, 0.1 eq.), tetrakis triphenylphosphine palladium (39 mg, 0.2 eq.), and potassium carbonate (41 mg, 3.0 eq.) were added, and the mixture was stirred at 100° C. for 24 hr. Upon the completion of the reaction, distilled water was added to the reaction solution, which was then extracted with ethyl acetate. The organic layer was washed with brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/methanol) to obtain the title compound (25 mg, 58%).

1. customUpon the completion of the reaction
2. distillationdistilled water
3. additionwas added to the reaction solution, which
4. extractionwas then extracted with ethyl acetate
5. washThe organic layer was washed with brine
6. dry with materialdried over sodium sulfate
7. customThe drying agent was removed by filtration
8. customthe residues obtained
9. concentrationafter concentration under reduced pressure
10. customwere purified by silica gel column chromatography (ethyl acetate/methanol)