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Herein, we present a convenient method of oxime ether synthesis in a one\u2010pot tandem electrochemical system using magnesium based metal\u2010organic framework\u2010derived magnesium oxide anchoring in self\u2010supporting carbon nanofiber membrane catalyst (MgO\u2010SCM), the <jats:italic>in situ<\/jats:italic> produced NH<jats:sub>2<\/jats:sub>OH from nitrogen oxides electrocatalytic reduction coupled with aldehyde to produce 4\u2010cyanobenzaldoxime with a selectivity of 93\u2009% and Faraday efficiency up to 65.1\u2009%, which further reacted with benzyl bromide to directly give oxime ether precipitate with a purity of 97\u2009% by convenient filtering separation. The high efficiency was attributed to the ultrafine MgO nanoparticles in MgO\u2010SCM, effectively inhibiting hydrogen evolution reaction and accelerating the production of NH<jats:sub>2<\/jats:sub>OH, which rapidly attacked carbonyl of aldehydes to form oximes, but hardly crossed the hydrogenation barrier of forming amines, thus leading to a high yield of oxime ether when coupling benzyl bromide nucleophilic reaction. This work highlights the importance of kinetic control in complex electrosynthetic organonitrogen system and demonstrates a green and safe alternative method for synthesis of organic nitrogen drug molecules.<\/jats:p>","DOI":"10.1002\/anie.202405553","type":"journal-article","created":{"date-parts":[[2024,4,9]],"date-time":"2024-04-09T22:39:35Z","timestamp":1712702375000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":40,"title":["Highly Efficient One\u2010pot Electrosynthesis of Oxime Ethers from NOx over Ultrafine MgO Nanoparticles Derived from Mg\u2010based Metal\u2010Organic Frameworks"],"prefix":"10.1002","volume":"63","author":[{"given":"Shihan","family":"Wang","sequence":"first","affiliation":[{"name":"Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education Lehn Institute of Functional Materials Institute of Green Chemistry and Molecular Engineering Guangdong Basic Research Center of Excellence for Functional Molecular Engineering School of Chemistry Sun Yat-Sen University  Guangzhou 510275 P.\u2005R. 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