应用正交设计法优化邻氯苯甲醚的合成工艺

Application of Orthogonal Design Method to Optimize the Synthesis of o-Chloroanisole

以邻氯苯酚（OCP）为原料,碳酸二甲酯（DMC）作甲基化试剂,在聚乙二醇-400（PEG-400）的催化下合成邻氯苯甲醚（OCA）,用正交设计法优化合成工艺,确定最佳工艺条件为n（PEG-400）∶n（OCP）∶n（DMC）∶n（K2CO3）=0.2∶1∶6∶0.001,反应温度为85-90℃,反应时间为10小时,邻氯苯甲醚的产率达到79%,经^1H-NMR和^13C-NMR确证其结构。改进后的工艺反应条件温和,操作安全简便,符合环境友好化学的发展方向,是一条切实可行的绿色合成工艺路线。

o-Chloroanisole was synthesized from o-Chlorophenol and dimethyl carbonate as methylating agent, PEG-400 as catalysts, technological condition was obtained with orthogonal design. To determine the best process conditions for n（PEG-400）∶n（OCP）∶n（DMC）∶n（K2CO3）=0.2∶1∶6∶0.001, reaction temperature is 85-90 ℃ and reaction time is 10 h, the yield of product reached 79 %. The target compound were confirmed by^ 1H-NMR and ^13C-NMR. Theimproved and optimized synthesis has more advantages such as mild reaction condition, technique is simple and safe. The developing direction which according with environmentally friendly chemistry is a feasible green synthetic route.