偏苯三酸酐酰氯的合成及其结构表征

以偏苯三酸酐(TMA)为反应原料、过量氯化亚砜作溶剂,二甲基甲酰胺(DMF)作催化剂制备了偏苯三酸酐酰氯(TMAC).利用三因素三水平正交实验研究了反应温度、反应时间、氯化亚砜用量3个因素对TMAC合成效率的影响并得到了优化工艺参数:反应温度70℃,反应时间7h,氯化亚砜用量为TMA质量的5倍时,TMAC的产率可高达96.47%.用红外图谱对化合物结构进行了确证:羧基特征峰完全消失,生成了相应的酰氯基团.该合成工艺可操作性强,提高了产物产率、纯度,反应速率,无副产物生成,可直接投入下步反应,对同类有机中间体获得更广泛的应用起到一定的作用.

Synthesis and structure characterization of trimellitic anhydride acid chloride

Trimellitic anhydride acid chlorid （TMAC） was prepared by using trimellitic anhydride （TMA）, thionyl anhydride as raw materials, and dimethyl formamide（DMF） as catalyst. The optimum preparation technology of TMAC was studied by orthogonal experiments of three facts and tree levels, and the optimum technological parameters are reaction temperature of 70℃, reaction time of 7 h, the quantity of thionyl anhydride 5 times the mass of TMA and the yield of TMAC of 96.47 %. The infra- red spectrum shows that carboxyl group peeks disappear, then the acid chloride group appear. In this synthetic method, the operability of the process gets better; the yield, the product purity and the reaction rate increase without by-products, which has reference effect on more widely application of this kind of organic intermediates.