In situ FT-IR and ex situ EPR analysis for the study of the electroreduction of carbon dioxide in N,N-dimethylformamide on a gold interface

Carbon monoxide, formate and carbonate were found as products from the CO2 reduction at a gold interface in DMF + TBAF solution. Carbonate could be formed also by reaction of CO2 with hydroxyl anions generated by reduction of the residual water in solution. The carbonate reacts with amines to form carbamates in good yields (72–96%). In situ FT-IR and ex situ EPR analysis have demonstrated the formation of free radicals in the absence of CO2 and at potentials more negative than −1.8 V (SCE). FT-IR measurements using s-polarized light have proved that these radicals are in solution. An electrochemical reaction of the electrolyte solution on the gold surface yielded a solid product involving particles from the gold surface.