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Herein, we report a photoelectrocatalytic strategy that bypasses these limitations by leveraging in situ\u2010generated nitrogen dioxide radicals (\u00b7NO\n                    <jats:sub>2<\/jats:sub>\n                    ) as homogeneous nitrating agents. Using a BiVO4 photoanode and nitrite as a sustainable nitrogen feedstock, \u00b7NO\n                    <jats:sub>2<\/jats:sub>\n                    radicals mediate the direct C\u2500H nitration of benzene via a radical aromatic substitution mechanism, obviating the need for reactant co\u2010adsorption. By engineering a polar interfacial layer on the photoanode, the local concentration of nitrite was remarkably enhanced, thereby boosting \u00b7NO2 generation and enabling efficient coupling even under practically relevant dilute conditions (5\u00a0mM NO\n                    <jats:sub>2<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    ). The optimized photoanode achieves a 29.6\u2010fold enhancement in p\u2010dinitrobenzene production rate over the unmodified BiVO4 and the scaled system further demonstrated a p\u2010DNB production rate of \u223c58\u00a0\u00b5mol\u00b7h\n                    <jats:sup>\u22121<\/jats:sup>\n                    with near exclusive selectivity and exceptional operational stability. This work establishes a waste valorization and sustainable platform for the synthesis of nitroaromatics from ambient conditions.\n                  <\/jats:p>","DOI":"10.1002\/anie.8746970","type":"journal-article","created":{"date-parts":[[2026,4,14]],"date-time":"2026-04-14T07:48:00Z","timestamp":1776152880000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Surface Polarity Reinforced Radicals Mediated C\u2500N Coupling Towards Photoelectrochemical Synthesis of Energetic Nitro Compounds"],"prefix":"10.1002","volume":"65","author":[{"given":"Chaoran","family":"Dong","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering Nanjing University of Science and Technology Nanjing 210094 China"},{"name":"Key Laboratory of Environmental Remediation and Ecological Health Ministry of Industry and Information Technology School of Environmental and Biological Engineering Nanjing University of Science and Technology Nanjing 210094 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cheng","family":"Lin","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Nanjing University of Science and Technology Nanjing 210094 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tianyu","family":"Wang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Environmental Remediation and Ecological Health Ministry of Industry and Information Technology School of Environmental and Biological Engineering Nanjing University of Science and Technology Nanjing 210094 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuhao","family":"Yang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Nanjing University of Science and Technology Nanjing 210094 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