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Mesoporous silica/graphene (KIT‐6/G) with pendent 3‐mercaptopropyl groups has been prepared by condensation of surface silanols and (3‐mercaptopropyl)trimethoxysilane (MPTMS). Treatment of the mercaptopropylated with Pd(CH3CN)2Cl2 gave a heterogeneous Pd‐catalyst (Pd@KIT‐6/G‐SH). The catalytic activity of the catalyst was investigated in two types of C−H functionalized for the synthesis of 2‐cyanoacetanilide and 2‐arylpyridine 1‐oxide derivatives via C−H activation. Additionally, for the study of the effect of thiol ligand, the Pd@KIT‐6/G was prepared from the treatment of Pd(CH3CN)2Cl2 with KIT‐6/G. The catalyst has been successfully recovered and reused without loss of activity over seven cycles of reactions.

A novel method for the palladium‐catalyzed decarboxylative ortho C–H bond arylation of pyridine 1‐oxides and anilides with benzoic acids as aryl sources is described. The established methodology provides a direct approach for the synthesis of 2‐arylpyridine 1‐oxides and 2‐aryl anilides in good isolated yields.

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