Abstract
Photoelectrocatalytic (PEC) strategy has emerged as a promising approach to drive organic reactions under mild conditions. Here, we present a protocol for PEC oxidative coupling of aromatic amines to produce aromatic azo compounds over a porous BiVO4 nanoarray (BiVO4-NA) photoanode. We describe the fabrication of BiVO4-NA photoanode and the detailed steps for the PEC oxidative coupling reaction, including key performance data of the BiVO4-NA photoanode for synthesizing azobenzene from aniline. For complete details on the use and execution of this protocol, please refer to Luo et al. (2022).1.