反应详情

温度

100 °C

Trifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl ester (Compound B1, 30 mg, 0.069 mmol) was dissolved in 1,4-dioxane (1 mL), added with thiomorpholine 1,1-dioxide (19 mg, 2 eq.), Pd2 (dba)3 (6.3 mg, 0.1 eq.), BINAP (8.6 mg, 0.2 eq.) and K3PO4 (29 mg, 2 eq.), and stirred at 100° C. overnight. The reaction solution was added to water, and then extracted with ethyl acetate. The organic layer was washed with saturated 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/hexane) to obtain the target compound (white powder, 2.1 mg, 7%).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over sodium sulfate
4. customThe drying agent was removed by filtration
5. customthe residues obtained
6. concentrationafter concentration under reduced pressure
7. customwere purified by silica gel column chromatography (ethyl acetate/hexane)
8. customto obtain the target compound (white powder, 2.1 mg, 7%)