CAJ | 학술논문

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-삼을양기규병기필정록화물시고재필정위양리자적리자액체필불가소적중간체,단시기현유적합성방법산솔저,지유약30%.문장연구료합성해중간체적계안화중반응온도、원료배비화세조용제대 N-삼을양기규병기필정록화물산솔적영향,실험결과표명:반응온도위130℃,γ-록병기삼을양기규완여필정적마이비위1∶1.7,후처리세조용제위을산을지시,N-삼을양기규병기필정록화물적수솔가이체도65%.선용을산을지작위반응후적세조용제,분층명현,대반응후잉여원료적세조거제효과호,대산품적순화유리.
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.