With 1,3-dichlorobenzene as raw materials, 2-chloro-1-(2,4-dichlorophenyl) ethanone (Ⅲ) was synthesized by Friedel-Crafts acylation, N-alkylation and oximation, then it was reacted with 2,4-dichlorobenzyl chloride and salinized by nitric acid, and got the final product oxiconazole nitrate (Ⅰ). The N-alkylation and oximation were performed by a "one-pot" reaction, and the key factors of the reaction were investigated. The improved synthetic route simplified the operation procedure, and the overall yield of oxiconazole nitrate was increased from 41.8% to 70.8%, with a purity of 99.9%.The structures of the products were characterized by IR, 1HNMR and HRMS spectra.