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Synthesis of oxime via the electrochemical method has potential advantages, accompanied by the upgrading of industrialization. Herein, we propose a novel strategy by introducing nickel (Ni) mediation to obtain high\u2010spin iron (Fe)(III) in phthalocyanine structure for synthesizing glyoxylate oxime via electrocatalytic nitric oxide (NO) coupling with keto acid. The optimized pFeNiPc catalyst achieved a Faradaic efficiency of 84.3% and a long\u2010term stability for glyoxylate oxime electrosynthesis. Moreover, the oxime could be directly cyclized to synthesize a gram\u2010level agrochemical isoxazoline molecule. The enriched amounts of high\u2010spin Fe(III) sites promote the accumulation of NO on the catalyst surface and further accelerate reduction, which enables the efficient adsorption\u2010conversion of NO to oxime. 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