Aminoxyl-mediated electrocatalysis offers a sustainable approach for the oxidation of alcohols to carboxylic acids. However, the high dosage of aminoxyl radicals and the limiting current density hinder the practicality of industrial application. Herein, a nickel-based electrocatalyst (Ni-tpdc) was synthesized on a three-dimensional porous graphite felt substrate. Taking advantage of the synergistic effect of the electrochemically activated Ni-tpdc/GF electrocatalyst with 4-acetamido-TEMPO, the yield of 4-pyridinecarboxylic acid was up to 99% with only 1 mol% ACT. A series of in situ measurements showed that NiOOH enhanced the activity of the intrinsic electrocatalyst. In addition, the synergistic system was extended to the oxidation of various heterocyclic alcohols. The scale-up synthesis of chiral acid (LEV-CO₂H) was achieved in an improved electrolyzer with a yield of 95.4%, enantiomeric retention of 99.2%, and space–time yield of 34.12 kg/m³ h. The practicality and effectiveness of this synergistic electrocatalytic strategy in practical electrosynthesis was further demonstrated.

中文翻译：

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通过 MOF 衍生的 NiOOH 促进低用量氨氧基杂环醇的电催化氧化


氨氧基介导的电催化为醇氧化成羧酸提供了一种可持续的方法。然而，氨氧基自由基的高剂量和极限电流密度阻碍了工业应用的实用性。在此，在三维多孔石墨毡基底上合成了镍基电催化剂（Ni-tpdc）。利用电化学活化的Ni-tpdc/GF电催化剂与4-乙酰氨基-TEMPO的协同效应，仅用1 mol% ACT，4-吡啶甲酸的产率就高达99%。一系列原位测量表明 NiOOH 增强了本征电催化剂的活性。此外，该协同系统还扩展到各种杂环醇的氧化。在改进的电解槽中实现了手性酸（LEV-CO ₂ H）的放大合成，产率达到95.4%，对映体保留率为99.2%，时空产率为34.12 kg/m ³ h。这种协同电催化策略在实际电合成中的实用性和有效性得到了进一步证明。