Abstract
Formation of a pre‐monolayer of a slightly soluble metal hydroxo complexes on electrode surface facilitates the electrooxidation. This factor, together with establishment of equilibria between the aldehyde and a geminal diol anion (which is the electroactive form) play important roles in electrooxidation of aromatic aldehydes. Better understanding of chemical and electrochemical processes involved, enables application of electroanalytical methods for investigation of reactions of orthophthalaldehyde—an important analytical reagent—in alkaline solution.