固载吡啶离子液体中间体：N-三乙氧基硅丙基吡啶氯化物的合成

摘要

N-三乙氧基硅丙基吡啶氯化物是固载吡啶为阳离子的离子液体必不可少的中间体，但是其现有的合成方法产率低，只有约30%。文章研究了合成该中间体的季铵化中反应温度、原料配比和洗涤溶剂对 N-三乙氧基硅丙基吡啶氯化物产率的影响，实验结果表明：反应温度为130℃，γ-氯丙基三乙氧基硅烷与吡啶的摩尔比为1∶1.7，后处理洗涤溶剂为乙酸乙酯时，N-三乙氧基硅丙基吡啶氯化物的收率可以达到65%。选用乙酸乙酯作为反应后的洗涤溶剂，分层明显，对反应后剩余原料的洗涤去除效果好，对产品的纯化有利。%N-[(triethoxysilyl)propyl]pyridinium chloride is indspensable intermediates in the preparation of supported pyridinium ionic liquids. However, the existing synthesis method gives a low yield, only about 30 %. In the paper, the effect of the reaction temperature, the ratio of raw materials in the reaction quaterisation, and solvents in work-up procedure on the yields of N-[(triethoxysilyl)propyl]pyridinium chloride were tested. The results showed that when the reaction temperature at 130 ℃, with a 1:1.7 molar ratio of γ-chloropropyl-triethoxysilane and pyridine, the yield of N-[(triethoxysilyl)propyl]pyridinium chloride reached 65 %. Using ethyl acetate as the cleaning solvent in work up, not only a obvious separation between light phase and dense phase was achieved, but also residual reactants could be removed.