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A rapid three-component cascade reaction for the synthesis of unsymmetric azo compounds via a radical activation strategy has been reported. Various aryldiazonium salts and unactivated alkenes are well compatible, providing the corresponding products in good to excellent yields. This strategy gives an efficient and practical solution for the synthesis of unsymmetric azo compounds with two C–N bond formation. A free radical pathway mechanism is advised for this transformation.

Graphical abstract: Hypervalent iodine(iii)-promoted rapid cascade reaction for the synthesis of unsymmetric azo compounds

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