反应详情

DCM (0.34 ml) solution of 8-methoxy-10,10-dimethyl-10H-11-oxa-2-aza-benzo[b]fluoren-5-one (Compound GT15-11, 10 mg) was cooled to −78° C., added with the DCM solution (0.17 ml) of 1.0 M BBr3, and the mixture was stirred at room temperature overnight. To the reaction mixture, water and saturated aqueous solution of sodium bicarbonate were added, and the solid produced therefrom was filtered off. The filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=9:1). The organic layer was washed with saturated brine. The filtered solid and the residues obtained after concentration under reduced pressure were combined to obtain the title compound (9.5 mg, 99%).

1. customthe solid produced
2. filtrationtherefrom was filtered off
3. extractionThe filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=9:1)
4. washThe organic layer was washed with saturated brine
5. customThe filtered solid and the residues obtained
6. concentrationafter concentration under reduced pressure