The synthesis of ethyl glyoxylate was studied by ozonization and hydro-reduction using diethyl maleate as raw material and ethyl acetate as solvent. The obtained optimum conditions were n(ethyl acetate):n(diethyl maleate)=15:1, ozonization temperature 20℃, ozonization time 80min; using Pa/C as hydrogenation catalyst, m(Pd/C):m(diethyl maleate)=0.09:1, hydrogen pressure 4MPa, reduction time 5h, reduction temperature 25 ℃. Under above conditions, the conversion of diethyl maleate was almost 100%, the yield of ethyl glyoxylate was ≥89.0% with the purity over 96.6%. The structure of obtained product was characterized by IR and 1H NMR.