A compact, high surface area nanostructured poly(2,5-dimethoxyaniline) powder having high electrical conductivity (σ∼ 10−1 S cm−1) and high charge storage capacity (Csp∼205 F/g) is synthesized in one step by chemical oxidative polymerization of 2,5-dimethoxyaniline using HCl/NaCl/H2O2 as a mild oxidizing system.