Polyester type dendrimers have been synthesized up to third generation using 4-[N,N-bis(2-hydroxyethyl)amino]-3-methoxy-4’-nitroazobenzene as core molecule and 3,5-bis[2-(tetrahydro-2H-pyran-2-yloxy)ethoxy]benzoic acid as branching unit. Growth of dendrimer was ensured by dicyclohexylcarbodiimide under catalysis of 4-N,N-dimethylaminopyridine in dry CH2Cl2, followed by deprotection of THP groups in EtOH/CH2Cl2 solution with HCl. Both steps give good yields decreasing with number of generation because of greater possibility of incomplete reactions with the growth of number of terminal groups.