Cyclic-voltammetric measurements show that 2-methylnaphthalene-1,4-diacetate is electrochemically oxidized on glassy-carbon electrode in glacial acetic acid at + 1.45V vs SCE. The process is irreversible and diffusion controlled. Preparative controlled-potential electrolysis indicates that 2-methyl-1,4-naphthoquinone is a sole product. The material and current yields of the process are 94 and 99%, respectively.