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Summary: Anilines are important feedstocks for pharmaceuticals, dyes, and other materials, but traditional approaches to their syntheses usually lack selectivity and environmental sustainability. Here, we describe the selective reduction of nitrobenzene to aniline under mild conditions, using water as the ultimate source of the required protons and electrons. We describe the electrochemical cell assembly, and detail steps for electrochemical reduction followed by organic extraction and analysis of the extracts using NMR.For complete details on the use and execution of this protocol, please refer to Stergiou and Symes (2022a). : Publisher’s note: Undertaking any experimental protocol requires adherence to local institutional guidelines for laboratory safety and ethics.