Description:
<jats:title>Abstract</jats:title><jats:p>Pyridine oximes produced from aldehyde or ketone with hydroxylamine (NH<jats:sub>2</jats:sub>OH) have been widely applied in pharmaceutics, enzymatic and sterilization. However, the important raw material NH<jats:sub>2</jats:sub>OH exhibits corrosive and unstable properties, leading to substantial energy consumption during storage and transportation. Herein, this work presents a novel method for directly synthesizing highly valuable pyridine oximes using in situ generated NH<jats:sub>2</jats:sub>OH from electrocatalytic NO reduction with well‐design nanofiber membranes (Al‐NFM) derived from NH<jats:sub>2</jats:sub>‐MIL‐53(Al). Particularly, 2‐pyridinealdoxime, the precursor of antidote pralidoxime (2‐PAM) for nerve agents suffering from scarcity and high cost, was achieved with a Faraday efficiency up to 49.8 % and a yield of 92.1 %, attributing to the high selectivity of NH<jats:sub>2</jats:sub>OH production on Al‐NFM, further easily reacted with iodomethane to produce 2‐PAM. This study proposes a creative approach, having wide universality for synthesizing pyridine and other oximes with a range of functional groups, which not only facilitates the conversion of exhaust gas (NO) and waste water (NO<jats:sub>2</jats:sub><jats:sup>−</jats:sup>) into valuable chemicals especially NH<jats:sub>2</jats:sub>OH production and in situ utilization through electrochemistry, but also holds significant potential for synthesis of neuro detoxifying drugs to humanity security.</jats:p>