Bis-[4-alquil/aril-5-tia-1,2,4-triazóis] foram preparados pela fusão de diácidos e tiosemicarbazidas, pela condensação de hidrazidas ácidas aromáticas com isotiocianato. A alquilação quimiosseletiva destes bis-[4-alquil/aril-5-tia-1,2,4-triazóis] com 1, -dihaloalcanos na presença de hidróxido de potássio em metanol aquoso, proporcionou N-alquil/aril tiatriazolofanos inéditos.Bis-[4-alkyl/aryl-5-thia-1,2,4-triazoles] were prepared by fusion of diacids and thiosemicarbazides by condensation of aromatic acid hydrazides with isothiocyanate. Chemoselective alkylation of these bis-[4-alkyl/aryl-5-thia-1,2,4-triazoles] with 1, -dihaloalkanes in presence of potassium hydroxide in aqueous methanol afforded novel N-alkyl/aryl thiatriazolophanes.