1-(3-Diethylaminophenyloxy)-2-propanol was synthesized with 3-hydroxy-N,N-diethylaniline and 1,2-propylene oxide as reactants. In the presence of alkaline catalyst, 1-(3-diethylaminophenyloxy)-2-propanol was synthesized. The effects of catalyst composition and preparation process on the catalytic synthesis of 1-(3-diethylaminophenyloxy)-2-propanol were investigated. The results showed that the MgO-Al2O3 composite oxides calcined at 300˚C exhibited efficient catalytic performance when the molar ratio of Mg:Al was 0.0015. The optimum reaction condition was as follows: reaction temperature 120˚C, reaction time 5 h, molar ratio of the reactants being n(3-hydroxy-N,N-diethylaniline):n(1,2-propylene oxide) = 1:1.7, and catalyst feeding ratio 1 wt%. Under the optimum reaction condition, the yield of 1-(3-diethylaminophenyloxy)-2-propanol reached 81.78%, the conversion rate was 93.06%, and the selectivity was 88.39%.