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A unique reactivity of zeolite based heterogeneous catalyst (ZSM‐5) is disclosed. ZSM‐5 in combination with NaNO2 resulted in direct access to nitriles by C−C cleavage of acetone derivatives at more substituted carbon. This cyanide free nitrile synthesis could be promising where one or more cyano‐labile electrophiles are present. Further, the catalyst has been successfully utilized for the synthesis of hydrazides from nitriles. Wide scope with high chemical yields have been achieved. Moreover, ZSM‐5 was recycled and reused several times without significant loss in its activity.

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