The development of a novel electrochemical methodology to generate carbon-11 carbon monoxide ([¹¹C]CO) from cyclotron-produced carbon-11 carbon dioxide ([¹¹C]CO₂) using Ni(cyclam) and Zn(cyclen) complexes is described. This methodology allows up to 10% yields of [¹¹C]CO from [¹¹C]CO₂. Produced [¹¹C]CO was subsequently converted to [¹¹C]N-benzylbenzamide under mild conditions with a radiochemical purity (RCP) of >98%.