m-chloroanisole was prepared from m-Chlorophenol in the presence of solid base and the phase transfer catalyst(PTC),using dimethyl carbonate(DMC) instead of dimethyl sulfate(DMS) as methylating reagent . The effect of solvent dosage, reactant mole ratio, reaction temperature and time on the conversion rate and yield of the product was studied. The optimum synthesis conditions were as follows through Response surface designs: Tetrabutyl ammonium bromide was used as PTC, Potassium carbonate was used as alkaline catalyst. n (m-Chlorophenol):n(DMC):n(Tetrabutyl ammonium bromide):n(Potassium carbonate)=1:3.83:1.07:0.5, reaction temperature 98oC, reaction time 7h. the yield of m-chloroanisole was 98.3% and the conversion rate of m-Chlorophenol was 100%.