一种新型的预偶联化合物的合成

Synthesis of a novel intermediate used in the preaminolysis procedure reaction

以乙烯基三氯硅烷、N,N′-二(1,1-二甲基乙醇)对苯二甲酰胺为原料,通过酰化、醇解及硅醚化反应合成了一种可用于“逐步偶联聚合方法”反应的偶联中间体,N,N′-二[1,1-二甲基-2-(乙烯基二氯)硅氧基乙基]对苯二甲酰胺(3)。其中两个1,1-二甲基亚乙基结构单元有效地增加了在有机溶剂中的溶解性,而四个Si—Cl键却使其对空气、水和酸都十分敏感。用甲醇与其进行醇解反应,可得到一种较稳定的化合物N,N′-二[1,1-二甲基-2-(乙烯基二甲氧基)硅氧基乙基]对苯二甲酰胺(4),其结构用红外光谱中的特征峰、核磁共振谱中质子的化学位移和数目、元素分析以及质谱进行了表征。

A novel intermediate N, N＇-di （1, 1-dimethyl-2- vinyldichlorosiloxylethyl） terephthaloyl amide （abbreviated as m ） in the first preaminolysis step of ＂Stepwise Coupling Polyefization＂ was first prepared from vinyhrichlorosilane and N, N＇-di（ 1,1-dimethylethanol）-terephthaloyl amide by acylation reaction, alcoholysis reaction and silicon etherification reaction. The 1,1-dimethylethylene in the intermediate can effectively enhance its solubility in organic solvents. The Si-Cl bonds in the intermediate 3 are hydrolytically unstable in the presence of air,water and acids. In order to separate the intermediate 3, the alcoholysis reaction of 3 with methanol,in which the relatively stable compound N, N＇-di （1,1-dimethyl-2-vinyldimethoxysiloxylethyl） terephthaloyl amide was obtained, has been used. The structure of the compound 4 was characterized by FTIR, 1HNMR, MS and Elemental analysis. The characterization results demonstrated that 4 possessed the proposed structure.