Abstract New 1, 2, 4-triazole-3-thiols were synthesized by reactions of the corresponding carboxylic acid hydrazides with isothiocyanates and subsequent cyclization of intermediate 1, 4-substituted thiosemicarbazides. Alkylation of 1, 2, 4-triazole-3-thiols with benzyl chlorides and bromacetophenones gave only S-substituted derivatives.