Department of Inorganic Chemistry, University of Madras, Guindy Campus, Chennai-600 025, India E-mail : vnnara@yahoo.co.in Annai Veilankanni’s College for Women (Arts and Science), Saidapet, Chennai-600 015, India Acyclic Schiff base was synthesized by microwave irradiation method. It was characterized by UV-Visible, FT-IR, and NMR spectroscopy techniques, the electrochemistry of the Schiff base was studied by cyclic voltammetry. The synthesized Schiff base was electrochemically polymerized, then used for electrochemical sensing of phenolic compounds. The polymerized Schiff base possesses high sensitivity towards the determination of phenolic compounds such as catechol, resorcinol and hydroquinone. The ability of polymerized Schiff base to form hydrogen bonding with phenolic compounds is one of the reasons for sensing of phenolic compounds at low potential. Polymerized acyclic Schiff base modified electrode shows better electrochemical sensing ability when compared to that of bare GCE.