反应详情

温度

210 °C

9-Bromo-3-chloro-8-methoxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound S1-4, 150 mg, 0.37 mMol) was dissolved in NMP, added with CuCN (100 mg, 3 eq.), and stirred at 210° C. for 1.5 hr under irradiation with microwave. After cooling, the reaction solution was added with water and ethyl acetate, and the precipitated solid was filtered to remove the solvent. The obtained residues were dissolved in DMF (1 ml), added with sodium azide (100 mg, 8 eq.) and ammonium chloride (5 mg), and then stirred at 120° C. for 24 hr in a sealed tube. After adding water, the insoluble matters were filtered and purified by HPLC to obtain the title compound (6.5 mg).

1. temperatureAfter cooling
2. filtrationthe precipitated solid was filtered
3. customto remove the solvent
4. dissolutionThe obtained residues were dissolved in DMF (1 ml)
5. stirringstirred at 120° C. for 24 hr in a sealed tube
6. filtrationthe insoluble matters were filtered
7. custompurified by HPLC