反应详情

Heat a mixture of 6-bromoisoquinoline (Aldrich; 0.320 g, 1.54 mmol), copper (I) iodide (0.155 g, 0.815 mmol), and potassium iodide (1.27 g, 7.96 mmol) in N,N-dimethylformamide (5.0 mL) to 130° C. at 3 h under microwave irradiation. Pour the cooled reaction mixture into 4:1 dichloromethane/diethyl ether (100 mL) and filter. Wash the filtrate with 5% aqueous sodium bisulfite solution (2×50 mL). Dry the organic layer over sodium chloride, decant the organic layer, and remove the solvents under reduced pressure. Dry the residue under vacuum for 18 h to give 0.4 g (100%) of the title compound as a dark red-brown solid. This material is carried on directly to the next step without further purification. MS (electrospray, m/z) 256.1 (M+1).

1. temperatureHeat
2. customunder microwave irradiation
3. additionPour
4. filtrationfilter
5. washWash the filtrate with 5% aqueous sodium bisulfite solution (2×50 mL)
6. dry with materialDry the organic layer over sodium chloride
7. customdecant the organic layer
8. customremove the solvents under reduced pressure
9. customDry the residue under vacuum for 18 h