By the condensation of 2,6-bis(4-amino-5-mercapto-[1,2,4]-triazoles-2)pyridine with aromatic acid in the presence of phosphorus oxychloride. Compounds of 2,6-bis(6-aryl-[1,2,4]-triazolo[3,4-b][1,3,4]-thiadiazole-3-yl)pyridines were synthesized. Their structures were confirmed by IR, 1H NMR spectroscopies and elemental analysis. Their electrochemical behavior and cyclic voltammogram also were be studied. The results showed that they have high ionization potentials and good affinity. The synthesis of 2,6-bis (4-amino-5-mercapto- [1,2,4] -triazoles-2) pyridine with aromatic acid in the presence of phosphorus oxychloride. Their structures were confirmed by IR, 1 H NMR spectroscopies and elemental analysis The electrochemical behavior and cyclic voltammogram also were be studied. The results showed that they have high ionization potentials and good affinity.