Camphoric anhydride was prepared by using camphoric acid as starting material and acetic anhydride as dehydrating agent. Then, ten novel camphoric acid-based diacylhydrazine compounds 3a～3j were synthesized by the N-acylation reaction of camphoric anhydride with aromatic acylhydrazines. The synthetic conditions were investigated preliminarily. The target compounds were characterized by means of FT-IR, 1H NMR, 13C NMR and ESI-MS techniques. The preliminary bioassay showed that, at the concentration of 50 mg/L, part of the title compounds exhibited good fungicidal activity, in which compound camphoric acid-based nicotinoyl hydrazine 3h had inhibition ratio of 96.3% against Physalospora piricola (better than that of the positive control azoxystrobin).