Visible‐Light Enabled Synthesis of 1‐Aryl‐3‐Sulfonylmethyl‐1,2,4‐Triazoles by Arylazo Sulfones

We present a novel and highly efficient method for synthesizing polyfunctionalized 1,2,4‐triazoles. This approach leverages visible light and arylazo sulfones in combination with N‐vinyl amides, in the environmentally friendly solvent ethyl acetate. Remarkably, the reaction proceeds without the need for (photo)catalysts, ensuring near‐perfect atom economy and producing only water as a by‐product. This method exhibits excellent functional group tolerance and can be scaled for both batch and continuous‐flow processes.