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Here, we report hydrogen peroxide generation at the 2‐nitrophenyloctyl ether (NPOE)/water interface with decamethylferrocene as an electron donor. The progress of this reaction was detected by the observation of a color change in the organic and aqueous phases in a series of shake‐flask experiments. The shape change in cyclic voltammograms recorded at a carbon‐paste electrode with decamethylferrocene in NPOE also indicates a (electro)catalytic reaction. Hydrogen peroxide was electrochemically detected at a Pt microelectrode tip positioned next to the carbon‐paste electrode. For this purpose, scanning electrochemical microscopy (SECM) approach curves were recorded. Analogous experiments demonstrated the possibility of electrochemical regeneration of the electron donor. The (electro)catalytic effect of MoS₂ on hydrogen peroxide generation was found by using both shake‐flask and SECM …