Highly efficient electrosynthesis of oximes from nitrates and carbonyl compounds in acidic media

Electrocatalytic nitrate reduction reaction (NO₃RR) coupled with organic compounds to synthesize oximes for value-added conversion of waste pollutants has very promising prospects. However, due to the susceptibility of the feedstock to hydrogenation, the relatively low reaction efficiency, and the poor stability of oximes, the reaction in acidic electrolytes remains a formidable challenge. Herein, we report a novel strategy for the one-step synthesis of oximes from nitrite and aldehydes/ketones in acidic electrolytes using a Zn-based catalyst (multilayered Zn nanosheet catalyst, M-ZnNSs). 99% yield and 99% selectivity of phenylacetaldehyde oxime were achieved at a constant current of −12 mA cm⁻². Moreover, various aldehydes/ketones were efficiently converted to oximes with yield and selectivity up to >90%, demonstrating the high versatility of this method. Furthermore, the catalyst exhibited remarkable long-term stability (>100 h). This work proposes a green strategy to promote the recycling of nitrogen resources, enhance the value of NO₃⁻ conversion products, and develop new ideas for electrochemical C-N coupling.