The synthetic approach toward ferrocenyl-terminated pyridylphenylene dendrimers based on tri- and tetrafunctional cores via the copper-catalyzed azide-alkyne cycloaddition is presented. Six dendrimers of three generations were synthesized and characterized using NMR spectroscopy, gel permeation chromatography (GPC), and elemental analysis. Cyclic voltammetry (CV) of the dendrimers shows a single quasi-reversible wave. The strong adsorption occurs onto Pt electrodes during CV studies in CH2Cl2 , which is reflected by the high i(pc)/i(pa) ratio. The modified electrodes coated with a ferrocenyl-terminated dendrimer of the second and third generations are stable toward CH2Cl2 washing and multiple CV scanning and proved to be able to sense Cu(+ )ions.