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The fundamental mechanism involves the generation of electron\u2013hole pairs in semiconductor photoelectrodes, where photogenerated holes drive oxidative transformations at the anode and electrons facilitate reductive reactions at the cathode. This approach enables precise control over reaction pathways under mild conditions, offering enhanced energy efficiency, improved selectivity and elimination of stoichiometric oxidants. This review comprehensively summarizes the rapid development of PEC organic synthesis, beginning with its fundamental principles and common photoelectrode fabrication techniques. Recent advances are then outlined across two major domains: the photoanode\u2010mediated oxidation of single molecules (e.g., alcohols, biomass\u2010derived platform chemicals, alkenes, and C\u2500H bonds) and photoelectrochemical cross\u2010coupling reactions for constructing C\u2500X (X\u00a0=\u00a0C, N, P, Cl, and Br) bonds. Finally, a forward\u2010looking perspective on critical challenges and future directions are discussed, which will significantly improve the insight for future development of PEC organic synthesis.<\/jats:p>","DOI":"10.1002\/anie.9133941","type":"journal-article","created":{"date-parts":[[2026,2,22]],"date-time":"2026-02-22T14:09:25Z","timestamp":1771769365000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Photoelectrochemical Heterogeneous Catalysis: From Single Molecule Oxidation Toward C\u2500X Bond Formation"],"prefix":"10.1002","volume":"65","author":[{"given":"Jinghao","family":"Wang","sequence":"first","affiliation":[{"name":"Chinese Academy of Science (CAS) Key Laboratory of Nanosystem and Hierarchy Fabrication CAS Center for Excellence in Nanoscience National Center for Nanoscience and Technology  Beijing P.R. China"},{"name":"University of Chinese Academy of Sciences  Beijing P.R. 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