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A straightforward, simple and efficient method is described for the synthesis of pyrazolo[1,2-a][1,2,4]triazole derivates via one-pot three-component reaction between isocyanides, dialkyl acetylenedicarboxylate and 4-phenyl urazole (as a NH-acid) in acetone without using any catalyst at ambient temperature. This method offers several advantages such as high yield of products, easy work-up procedure and mild reaction conditions.