A variety of 5-aryl-2-methyltetrazoles and 5-aryl-2-benzyltetrazoles were directly prepared in good to moderate yields by the reaction of aromatic aldehydes with methylhydrazine and benzylhydrazine, followed by treatment with di-tert-butyl azodicarboxylate and [bis(trifluoroacetoxy)iodo]benzene in a mixture of dichloromethane and 2,2,2-trifluoroethanol at room temperature. The present method is a novel one-pot preparation of 5-aryl-2-methyltetrazoles and 5-aryl-2-benzyltetrazoles through a [2N + 2N] combination under transition metal-free and mild conditions.

Various diethyl 3‐arylisoxazole‐4,5‐dicarboxylates were efficiently prepared in good to moderate yields by the successive treatment of benzylic chlorides and alkyl p‐tosylates with N‐methylmorpholine N‐oxide (NMO) and then hydroxylamine hydrochloride and potassium carbonate followed by Oxone® and diethyl acetylenedicarboxylates. This one‐pot proccess was carried out under mild, transition‐metal‐free conditions.

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A novel one‐pot, two‐step preparation of 5‐aryltetrazoles from aromatic aldehydes and alkylhydrazines is presented.