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The one‐pot synthesis of a series of sulfonium salts containing transferable diazomethyl groups is described, and the structure of these compounds is elucidated by X‐ray crystallography. Under photochemical conditions, reaction of these salts with  N , N ‐dialkyl hydrazones affords 1‐(dialkylamino)‐1,2,3‐triazoles via diazomethyl radical addition to the azomethine carbon followed by intramolecular ring closure. The straightforward transformation of the structures thus obtained into mesoionic carbene–metal complexes is also reported and the donor properties of these new ligands characterized.

α‐Diazo Sulfonium Triflates: Synthesis, Structure, and Application to the Synthesis of 1‐(Dialkylamino)‐1,2,3‐triazoles