A series of β‐ketonitriles was synthesized within 30 min under mild conditions through the BF3·OEt2‐catalyzed addition reactions of diazoacetonitrile to aromatic aldehydes and subsequent 1,2‐hydride shift. This method is advantageous in that it is operationally simple, mild and metal‐free conditions are used, the substrate scope is wide, and the products are obtained in moderate to high yields (up to 81 %). Additionally, γ,δ‐unsaturated β‐ketonitriles are also accessible by this method by using cinnamaldehydes.

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Mild conditions and a short reaction time result in a successful preparation of the title compounds, required as important synthetic intermediates.