电化学Minisci反应实现N-聚芳烃烷基化

Diphenyl phosphate (25.0 mg, 1 equiv.), ammonium hexafluorophosphate (81.5 mg, 5 equiv.) and a magnetic stirrer were added to a 5 mL ElectraSyn vial. Reagents were dissolved in THF (2mL) and to the stirred solution were added 1 (0.1 mmol) and 2 (5 equiv.), followed by water (1mL). The vial was closed, reticulated vitreous carbon was used as working electrode and nickel foam as counter electrode, ElectraSyn 2.0 was set at constant current (10 mA) during 120 min. The crude mixture was then diluted with ethyl acetate, extracted with saturated aqueous solution of NaHCO3 (2 x 5 mL), washed with brine (3 x 30 mL), dried over anhydrous MgSO4, filtered and the solvent was evaporated under reduced pressure. The crude mixture was purified by flash column chromatography using silica gel and the eluent indicated in each case.

简要

General electrochemical Minisci alkylation of N-heteroarenes with alkyl halides；Roberto del Río-Rodríguez, Lorena Fragoso-Jarillo, Alberto F. Garrido-Castro, Carmen Maestro -Rubio, Jose A. Fernández-Salas,*and José Alemán*； Chem. Sci., 2022,13, 6512-6518。