An AB(2) monomer N,N-bis[2-(4-aminobenzoyloxy)ethyl]aniline was synthesized by nucleophilic substitution reaction between N,N-bis (2-chloroethyl)aniline and 4-aminobenzonic acid. Based on the monomer, the azo-coupling reaction was explored for the first time to prepare a hyperbranched azo polymer. The results showed that the scheme was a feasible way to synthesize hyperbranched azo polymers under extremely mild conditions.