微波辅助合成对羟基苯甲醚

Synthesis of 4-Methoxyphenol by Microwave-Assisted Method

以对苯二酚为原料、碳酸二甲酯(DMC)为甲基化试剂、聚乙二醇-400(PEG-400)为相转移催化剂,在微波辅助条件下合成对羟基苯甲醚,并通过1 HNMR对其结构进行了确证。通过正交实验确定最优合成条件为:n(对苯二酚)∶n(DMC)∶n(K2CO3)∶n(PEG-400)=1∶8∶0.65∶0.40、反应温度95℃、反应时间35min,在此条件下,对羟基苯甲醚的收率为76.40%。该合成方法避免了剧毒试剂的使用,安全性高,操作简单。

4-Methoxyphenol was synthesized by microwave-assisted method using hydroquinone as raw ma- terial,dimethyl carbonate（DMC） as methylating reagent, polyethylene glycol-400 （PEG-400） as phase transfer catalyst. And its structure was confirmed by 1 HNMR. Through orthogonal experiment,the optimum conditions were obtained as follows：n（hydroquinone） ： n（DMC） ： n（K2CO3） ： n（PEG-400） was 1 ： 8 ： 0.65 ： 0.40,reac- tion temperature was 95 ℃, reaction time was 35 min. Under above conditions, the yield of 4-methoxyphenol reached 76.40%. This synthetic method avoids the use of poisonous reagent,which is simple and safe.