Photoelectrocatalytic C-H halogenation over an oxygen vacancy-rich TiO<sub>2</sub> photoanode.

Li, Zhenhua; Luo, Lan; Li, Min; Chen, Wangsong; Liu, Yuguang; Yang, Jiangrong; Xu, Si-Min; Zhou, Hua et al. · Nat Commun · 2021

basic_science · Level V

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Abstract

Photoelectrochemical cells are emerging as powerful tools for organic synthesis. However, they have rarely been explored for C-H halogenation to produce organic halides of industrial and medicinal importance. Here we report a photoelectrocatalytic strategy for C-H halogenation using an oxygen-vacancy-rich TiO<sub>2</sub> photoanode with NaX (X=Cl<sup>-</sup>, Br<sup>-</sup>, I<sup>-</sup>). Under illumination, the photogenerated holes in TiO<sub>2</sub> oxidize the halide ions to corresponding radicals or X<sub>2</sub>, which then react with the substrates to yield organic halides. The PEC C-H halogenation strategy exhibits broad substrate scope, including arenes, heteroarenes, nonpolar cycloalkanes, and aliphatic hydrocarbons. Experimental and theoretical data reveal that the oxygen vacancy on TiO<sub>2</sub> facilitates the photo-induced carriers separation efficiency and more importantly, promotes halide ions adsorption with intermediary strength and hence increases the activity. Moreover, we designed a self-powered PEC system and directly utilised seawater as both the electrolyte and chloride ions source, attaining chlorocyclohexane productivity of 412 µmol h<sup>-1</sup> coupled with H<sub>2</sub> productivity of 9.2 mL h<sup>-1</sup>, thus achieving a promising way to use solar for upcycling halogen in ocean resource into valuable organic halides.