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采用碳酸二甲酯(DMC)代替传统的有毒有害试剂作甲基化试剂,以2,6-二氯苯酚(DCP)为原料,在固体碱与相转移催化剂(PTC)作用下,合成了2,6-二氯苯甲醚(DCA)。考察了PTC种类及用量、物料配比、反应时间、反应温度和碱性催化剂用量对反应的影响,得到最佳反应条件为:以聚乙二醇400(PEG-400)为PTC,x(PEG-400)=0.2%,n(DMC)∶n(DCP)∶n(K2CO3)=0.1∶0.05∶0.003,温度150℃,时间5h,在该条件下,DCA的收率为87.3%,DCP的转化率为100%。优化条件下的重复实验表明,该反应易于控制,重复性好。
Using dimethyl carbonate (DMC) instead of traditional toxic and hazardous reagents as methylation reagent and 2,6-dichlorophenol (DCP) as raw materials, the reaction of solid base with phase transfer catalyst (PTC) , 6-dichloroanisole (DCA). The effects of the type and amount of PTC, the ratio of materials, the reaction time, the reaction temperature and the amount of basic catalyst on the reaction were investigated. The optimal reaction conditions were: PEG (PEG-400) (DMC): n (DCP): n (K2CO3) = 0.1: 0.05: 0.003, temperature 150 ℃ and time 5h, the yield of DCA was 87.3% Conversion is 100%. Repeated experiments under optimized conditions showed that the reaction was easy to control and reproducible.