A novel method was developed for the synthesis of N-alkoxyacylimidoyl halide by the reaction of α-nitro ketone and alkyl halides in the presence of NaHSO 4 /SiO 2 . Nitrile oxides that are generated from αnitro ketones by silica gel supported acid catalysts are the possible intermediate, which react with alkyl halides to form N-alkoxyacylimidoyl halides. Novel 17 N-alkoxyacylimidoyl halides were synthesized by this procedure.
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