The electrochemical generation of highly active and variable free radicals for the synthesis of organic compounds has emerged as a favored approach due to its mild and environmentally friendly characteristics, in contrast to traditional chemical redox reagents. As such, electrochemistry has been extensively applied in a wide range of synthetic transformations for the construction and functionalization of N/S-heterocycles in recent years. In this review, we present a comprehensive overview of our recent advancements in the methodology of electrochemically assisted radical generation and its subsequent application in the synthesis and functionalization of diverse N/S-heterocyclic compounds. In practice, we have developed various methodologies for the functionalization of N/S-heterocyclic compounds, including thiocyanation, alkylation, sulfonation, hydrogenation, pyridination, and the synthesis of complex N/S-containing heterocyclic compounds from readily available starting materials in an undivided cell. The methodology and mechanism of electrochemically mediated synthesis and functionalization of N/S-heterocycles will be discussed in terms of direct anodic oxidation, indirect oxidation, cathodic reduction, and paired electrolysis.
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