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<p>Activating benzylic C(sp<sup>3</sup>)–H bonds is essential in organic synthesis. However, electrocatalytic oxidation of methyl arenes to aromatic aldehydes remains challenging, particularly under aqueous electrolysis conditions. In this work, we have confirmed CoO<sub>2</sub> as the active phase for the electrochemical methyl arene oxidation reaction on Co-based catalysts through theoretical calculations, and propose oxygen-vacancy-rich Co<sub>3</sub>O<sub>4</sub> for efficient electrochemical methyl arene oxidation reaction performances. The generation of CoO<sub>2−<i>x</i></sub> species is extremely difficult for Co<sub>3</sub>O<sub>4</sub>, so that it is almost inactive for the electrochemical methyl arene oxidation reaction on Co<sub>3</sub>O<sub>4</sub>. Through a combination of <i>in/ex situ</i> characterizations, we proved that oxygen vacancy could induce the electrochemical reconstruction of Vo-Co<sub>3</sub>O<sub>4</sub> to CoO<sub>2−<i>x</i></sub> species on the catalyst surface for achieving excellent electrochemical methyl arene oxidation reaction performance, and the aromatic aldehyde yield and the Faraday efficiency are 90% and 40%, respectively, for electrochemical methyl arene oxidation reaction on Vo-Co<sub>3</sub>O<sub>4</sub>. This strategy enables the electrochemical methyl arene oxidation reaction to proceed efficiently under predominantly aqueous conditions, providing an efficient and sustainable method for aromatic aldehyde synthesis.</p>

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Oxygen vacancy induced aqueous electrosynthesis of aromatic aldehydes from benzylic C(sp3)–H

  • 期刊论文

  • 发表日期：

    2026年7月24日

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  • Yimin Jiang,
  • Wei Chen,
  • Xichang Liu,
  • Mengwei Han,
  • Chao Xie,
  • Yandong Wu,
  • Ruiqi Wang,
  • Junhao He,
  • Yuqin Zou,
  • Shuangyin Wang

摘要

Activating benzylic C(sp3)–H bonds is essential in organic synthesis. However, electrocatalytic oxidation of methyl arenes to aromatic aldehydes remains challenging, particularly under aqueous electrolysis conditions. In this work, we have confirmed CoO2 as the active phase for the electrochemical methyl arene oxidation reaction on Co-based catalysts through theoretical calculations, and propose oxygen-vacancy-rich Co3O4 for efficient electrochemical methyl arene oxidation reaction performances. The generation of CoO2−x species is extremely difficult for Co3O4, so that it is almost inactive for the electrochemical methyl arene oxidation reaction on Co3O4. Through a combination of in/ex situ characterizations, we proved that oxygen vacancy could induce the electrochemical reconstruction of Vo-Co3O4 to CoO2−x species on the catalyst surface for achieving excellent electrochemical methyl arene oxidation reaction performance, and the aromatic aldehyde yield and the Faraday efficiency are 90% and 40%, respectively, for electrochemical methyl arene oxidation reaction on Vo-Co3O4. This strategy enables the electrochemical methyl arene oxidation reaction to proceed efficiently under predominantly aqueous conditions, providing an efficient and sustainable method for aromatic aldehyde synthesis.