Yi Zhou, Chaofan Wan, Qizhi Min, Xuan Wu, Ping Zhu, Y W Sun, Wenhua Zhang, Jie Yang
ABSTRACT The electrocatalytic synthesis of glycine from oxalic acid (H 2 C 2 O 4 ) and hydroxylamine (NH 2 OH) involves a complex multi‐step pathway comprising C–N coupling and multi‐step selective protonation, making rational catalyst design a major challenge. In this work, by combining constant‐potential density functional theory (DFT), the reaction mechanisms for the formation of glyoxylic oxime (GAO) from H 2 C 2 O 4 and NH 2 OH on Pb surfaces, and its subsequent reduction to glycine on Cu surfaces are revealed. Guided by these mechanistic insights, we propose a set of criteria for designing integrated dual‐site catalysts capable of catalyzing both GAO formation and selective protonation to glycine. Among the theoretically screened out integrated Pt 1 (Ir 1 , Ru 1 )/Pb(100) single atom catalysts, Pt 1 /Pb catalyst is synthesized experimentally, demonstrating high activity for glycine production. This study bridges fundamental mechanistic understanding with practical catalyst development for complex multi‐step electrosynthesis.