A scalable Ni- or Ni/Pd-catalyzed electrochemical reductive coupling method is disclosed, affording biaryls in good to excellent yield via the electrolysis of lignin-derived aryl sulfonate esters. This method features the enhanced reactivity provided by the combination of transition metal catalysis and electrochemistry and the high selectivity for desired biaryls over other side products. The biaryls find applications in building blocks for high-performance polyesters or PVC plasticizers.