A novel and efficient one-pot method has been developed for the synthesis of 2-amino-1,3,4-thiadiazoles using various carboxylic acid hydrazides with trimethylsilyl isothiocyanate (TMSNCS). In situ preparation of various thiosemicarbazides by the reaction of different carboxylic acid hydrazides with trimethylsilyl isothiocyanate (TMSNCS), followed by cyclodehydration of thiosemicarbazides under acidic conditions gave 2-amino-1,3,4-thiadiazoles in high yields (71-87%).

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A new class of bicyclic silaheterocycles, 6,6‐dimethyl‐2‐aryl‐6,7‐dihydro‐5H‐[1,2,4]triazolo[5,1‐b][1,3,5]thiazasilines, which could be developed as potential sila‐drugs. The reactions of several 3‐aryl‐5‐mercapto‐1,2,4‐triazoles with bis(chloromethyl)dimethylsilane under basic conditions gave high yields of bicyclic products. Reaction, product workup and isolation were streamlined without requiring an anhydrous solvent, inert gas or chromatographic purification. The products were structurally characterized by single‐crystal X‐ray diffraction.