AZELAIC ACID MONOMETHYL ESTER was prepared by ozone oxidation using methyl oleate as a raw material and a mixture of acetic acid and n-hexane as a solvent. The synthesis conditions for AZELAIC ACID MONOMETHYL ESTER were: V(methyl oleate):V(mixed solvent) = 1:4, ozonation reaction temperature of 10–13 °C, oxidative pyrolysis temperature of 90–95 °C, and oxidative pyrolysis time of 2.5 h. The crude product was purified by molecular distillation. Under these conditions, the yield of AZELAIC ACID MONOMETHYL ESTER was ≥78%, and the purity was ≥96%.