We applied the hysteresis-based descriptor to closed-loop autonomous kinetic investigations of the TEMPO-catalyzed alcohol electro-oxidation reaction shown in Scheme 2. Here, TEMPO (precursor R) is oxidized at the electrode to generate TEMPO + which acts as catalyst (O), reacting with a primary or secondary alcohol (S) to convert them to the corresponding aldehydes or ketones. This catalytic reaction regenerates TEMPO by either an additional electron transfer step or a comproportionation step which are fast. Overall, the reaction in Scheme 2 is of practical interest for organic electrosynthesis and biomass valorization. Scheme 2. Mechanism of TEMPO-catalyzed alcohol electro-oxidation. Ethanol and isopropanol were studied as substrates in this work.