Electrochemical Laboratory of Green Synthesis, Department of Chemistry, University of Allahabad, Allahabad-211 002, Uttar Ptadesh, India E-mail : rkp.singh@rediffmail.com Manuscript received 18 May 2009, revised 11 August 2010, accepted 30 August 2010 The electrochemical methoxylation of 4-chlorobenzaldehyde, 4-hydroxybenzaldehyde, 4-anisylaldehyde and 4,4- N,N'-dimethylaminobenzaldehyde was carried out at platinum electrode. Constant potential electrolysis was carried out in undivided electrochemical cell. The reaction is an example of nuclear oxidation of aromatic compounds with substitution. The experimental parameters involved in the reaction are discussed here.