A process for the microfluidic electrochemical synthesis of geminal dipseudohalide or halide-pseudohalide compounds comprising the steps of pumping a solution comprising a compound of Formula I ##STR00001## into a microfluidic electrochemical reactor in the presence of a base, one of a halide or pseudohalide salt (MY), and a mediator; applying an electrical current through the microfluidic electrochemical reactor; and performing oxidative addition to create a geminal dipseudohalide or halide-pseudohalide compound of the general Formula II ##STR00002##