Marmara University, Faculty of Pharmacy, Department of Pharmaceutical Chemistry, Istanbul, Turkey DOI : 10.12991/2013171313 3,4-Disubstituted-2,4-dihydro-5H-1,2,4-triazole-5-thiones were synthesized by a new one-pot, two-step synthesis method which was demonstrated to be superior than the current synthesis methods. The new method involves addition of alkyl/aryl isothiocyanates to substituted hydrazides in ethanol following the refluxing process of intermeadiate in 4N sodium hydroxide solution. According to our new synthesis procedure, reaction has gone to completion within 6 hours by higher product yields and reduced solvent usage. Keywords : 1,2,4-triazole-5-thione, synthesis, method development