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Device-level applications of organic electrolytes unavoidably imply extensive contacts with the environment. Despite their excellent scientific potential, ionic liquids (ILs) cannot be approved for practical usage until their life cycle...

Investigation of catalytic reactions using nuclear magnetic resonance (NMR) is a crucial task, which is often challenging to perform due to rather complex transformations at the metal center. In this work, it was shown that electrophoretic NMR can be a suitable method for studying catalytic reactions and for observing the changes in the catalyst nature. As an important example involving palladium catalysts with N‐heterocyclic carbine ligands (NHCs), the breakage of the Pd‐NHC bond can occur during the catalytic process. Electrophoretic NMR allows the distinction of compounds in the spectra depending on the charge, thus bringing new opportunities to mechanistic studies. Here, we present independent evidence of R‐NHC product formation in the Pd‐catalyzed Mizoroki–Heck reaction—the key process for catalyst change from the molecular to nano‐scale type.