da 4-amino-2-metilquinolina foram sintetizados. Suas estruturas químicas foram caracterizadas e confirmadas através de análise elementar, espectroscopia no infravermelho (IR), ressonância magnética nuclear (RMN) de 1 H e espectrometria de massas (MS). O comportamento eletroquímico do composto de partida (4-amino-2-metilquinolina) e dos dois azo-derivativos sintetizados foi estudado com um eletrodo de mercúrio em solução tampão universal B-R em diferentes valores de pH (2-11,5) contendo etanol 40% (v/v) usando polarografia dc, voltametria cíclica e coulometria com potencial controlado. Os caminhos de reação dos compostos no eletrodo foram elucidados e são discutidos. As constantes de dissociação (pKa) dos compostos examinados, constantes de estabilidade e estequiometria dos complexos formados em soluções dos compostos com alguns íons de metais de transição (Co(II), Ni(II), Cu(II), La(III) and UO 2 2+ ) foram determinadas.Two azo-compounds, 2-methyl-4-(5-amino-2-hydroxy-phenylazo)-quinoline (2) and 2-methyl-4-(2-hydroxy-5-nitrophenylazo)-quinoline, derived from 4-amino-2-methylquinoline were synthesized. Their chemical structures were characterized and confirmed by means of elemental chemical analysis, infrared (IR) spectroscopy, 1 H nuclear magnetic resonance (NMR) and mass spectrometry (MS). The electrochemical behavior of the starting compound (4-amino-2-methylquinoline) and of the two synthesized azo-derivatives was studied at the mercury electrode in the B-R universal buffer at various pH values (2-11.5) containing 40% (v/v) ethanol using dc-polarography, cyclic voltammetry and controlled-potential coulometry. Their electrode reaction pathways were elucidated and discussed. The dissociation constants (pKa) of the examined compounds, stability constants and stoichiometry of their complexes in solution with some transition metal ions (Co(II), Ni(II), Cu(II), La(III) and UO 2 2+ ) were determined.