2,6-dichloroanisole(DCA) was prepared from 2,6-dichlorophenol(DCP) in the presence of potassium carbonate (K2CO3) and phase transfer catalyt(PTC), using dimethyl carbonate (DMC) as methylating reagent instead of conventional toxic reagents. The best yield(87.3%) of DCA and conversion (100%) of DCP were obtained under optimized conditions that polyethylene glycol 400 (PEG-400) was used as PTC, x(PEG-400)=0.2%, n(DMC):n(DCP):n(K2CO3)=0.1:0.05:0.001, the reaction temperature 150 oC, the reaction time 5 h. The repeat experiments showed that the technology possed a good repeatability under above optimum conditions.