1,2,3-三甲氧基苯的绿色合成

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),行用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~1H NMR方法对产物进行了分析和表征。

Green Synthesis of 1,2,3-Trimethoxybenzene

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(Bmiml Br)as the catalyst,which was prepared from butyl- bromide and N-methylimidazolium and was characterized by means of FTIR and~1H 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(BmimlBr):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.