We report herein a one-pot synthesis of unsymmetrical disulfides with trichloroisocyanuric acid (TCCA) as an oxidant. Under facile conditions, aromatic-aromatic disulfides and aromatic-aliphatic disulfides were synthesized in good to excellent yields even without base. For the construction of the challenging aliphatic-aliphatic disulfides, good yields of the desired products were also obtained with slightly modified conditions. Additionally, the reactions demonstrated a wide range of substrate scope, very short reaction time (<5 min), and convenient procedures. (C) 2016 Elsevier Ltd. All rights reserved.