Aryl Triazenes From N , N ‐Dialkylformamide and Aryldiazonium Salts

Triazenes are valuable nitrogen‐containing motifs with applications in medicinal and synthetic chemistry. Herein, we report a simple and efficient room‐temperature synthesis of 1‐aryl‐3,3‐dialkyl triazenes using N , N ‐dialkylformamides as both solvent and dialkylamine source. The transformation proceeds under mild conditions with broad functional‐group tolerance, including heteroaryl substrates, affording the desired triazenes in moderate to good yields. Mechanistic investigations suggest a nucleophilic attack of N , N ‐dialkylformamide on diazonium salts through the O atom, followed by deformylation, with formic acid and acetic acid identified as byproducts. The synthetic utility of the protocol is further demonstrated through gram‐scale synthesis. This operationally simple and scalable method offers a practical approach for the preparation of structurally diverse triazenes.