1,2,3-三甲氧基苯的绿色合成

Green Synthesis of 1,2,3-Trimethoxybenzene

采用一步法用溴代正丁烷和N-甲基咪唑制备了离子液体1-丁基-3-甲基咪唑溴化物（[Bmim]Br），并用FTIR和^1H NMR方法对其结构进行了表征。在[Bmim]Br催化作用下，以碳酸二甲酯（DMC）为甲基化试剂、焦性没食子酸（PA）为原料合成了连1，2，3-三甲氧基苯（TMB），并通过正交实验考察了反应温度、反应时间、原料配比及[Bmim]Br用量等因素对合成反应的影响。实验结果表明，合成TMB的适宜反应条件为：反应温度160℃、n（PA）：n（DMC）=1：6、反应时间7h、n（[Bmim]Br）：n（PA）=1：1。在此条件下，PA转化率为100．0％，TMB收率为92．60％。用GC—MS和’HNMR方法对产物进行了分析和表征。

1,2,3-Trimethoxybenzene（TMB） was synthesized from pyrogallic acid（PA） and dimethyl carbonate （DMC） as methylating reagent instead of the conventional toxic reagents with ionic liquid 1-butyl-3-methylimidazolium bromide （[Bmim] Br） as the catalyst, which was prepared from butyl-bromide and N-methylimidazolium and was characterized by means of FTIR and ^1 H NMR. Orthogonal experiments were conducted to optimize the reaction conditions. The results showed that under the optimized reaction conditions of reaction temperature 160 ℃, mole ratio of PA to DMC 1 ： 6, reaction time 7 h and n（[Bmim]Br） ： n（PA） 1 ： 1, conversion of PA and yield of TMB reached 100.0% and 92.60%, respectively. The product TMB was corroborated by means of GC-MS and ^1H NMR.