3,5-disubstituted-1,2,4-tiadiazoles with substituted-styril and heterocycle-vinyl were obtained by extending the method which implies the use of 3,5-disubstituted-1,2,4-ditiazolium salts as precursors [1-4]. A comparative study of the reaction process in the case of perchlorates, diacide phosphates, tribromides and 3,5-distyrile-dithiazolium triiodides, taken as etalon, was perfomed. Good yields were obtained when using perchlorates, phosphates and triiodides. The reaction was made by heating the reaction mixture and by ultrasound exposure. The structure of the compounds was confirmed by chemical and physical analysis and the data obtained were identical to those of 3,5-disubstituted-1,2,4-tiadiazoles obtained by another methods [5,6]. The biological (antibacterial and anticancer) activity of the synthesized compounds was tested and the results indicated a medium activity.