A redox active ionic liquid (RIL), 1-ethyl-4-(methoxycarbonyl)pyridinium bis(fluorosulfonyl)amide with a half unit of methyl viologen, was synthesized from its iodide form by anion exchange reaction and were characterized by NMR, UV-VIS, IR and elemental analysis. The compound exhibited redox waves in CH3CN with or without n-Bu4NPF6 electrolyte at -0.76 and -1.55 V vs. Ag/AgCl attributed to RIL to its radical form (RIL •) and RIL • to its anion form (RIL- ), respectively. The redox behavior indicates the dual role of the ionic liquid as a solvent and electrolyte. The redox wave RILs was also observed in neat condition without any additional solvent and electrolyte using micro-electrode. The cyclic voltammogram (CV) of RILs changed dramatically in the presence of acetic acid to show proton-coupled electron transfer (PCET) process for proton reduction at -1.33 V vs. Ag/AgCl in CH3CN. The change in CV indicates that RIL could act as a catalyst for hydrogen (H2) production via RIL-H as shown in Scheme 1. The bulk electrolysis of acetic acid with RILproduced H2 with 13.4 turnover number based on RIL and current yield of 37.8 %. In addition, the electrolysis for H2generation proceeded in complete ionic liquid system of RIL. The RIL could work as catalyst, electrolyte, and solvent for H2 production. Figure 1
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