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1-甲基咪唑醋酸离子液体催化合成甲基丙烯醛
引用本文:王奇伟,高明.1-甲基咪唑醋酸离子液体催化合成甲基丙烯醛[J].浙江化工,2014(11):22-25.
作者姓名:王奇伟  高明
作者单位:浙江震元制药有限公司
摘    要:合成了1-甲基咪唑醋酸(Mim]Ac)质子型离子液体,对其进行了1H NMR和IR表征。以Mim]Ac为催化剂,甲醛、丙醛、二乙胺为原料,通过Mannich反应制备了甲基丙烯醛。考察了原料投料比、Mim]Ac用量、Mannich反应温度和反应时间等因素对甲基丙烯醛收率的影响。研究结果表明,当甲醛、丙醛和二乙胺的摩尔比为1.1:1.0:1.0,Mim]Ac用量(物质的量)为丙醛的10.0%,Mannich反应温度为45℃,反应时间为50 min,分解反应温度为75℃,甲基丙烯醛的收率为95.3%,并对产物进行了1H NMR表征。同时,对Mim]Ac质子型离子液体催化Mannich反应的机理进行了初步研究。

关 键 词:离子液体  甲基丙烯醛  Mannich反应

Synthesis of Methacrolein Catalyzed by 1-Methylimidazolium Acetate Ionic Liquid
WANG Qi-wei,GAO Ming.Synthesis of Methacrolein Catalyzed by 1-Methylimidazolium Acetate Ionic Liquid[J].Zhejiang Chemical Industry,2014(11):22-25.
Authors:WANG Qi-wei  GAO Ming
Affiliation:(Zhejiang Zhenyuan Pharmaceutical Co., Ltd., Shaoxing, Zhejiang 312000, China)
Abstract:1-Methylimidazolium acetate (Mim]Ac) protic ionic liquid was prepared, and its structure was confirmed by 1H NMR and IR. Methacrolein was prepared through Mannich reaction of formaldehyde, propionaldehyde, and diethyl amine with Mim]Ac as the catalyst. The influences of molar ratio of reactants, amount of catalyst, Mannich reaction temperature and reaction time were investigated. The proper reaction conditions were as follows: the molar ratio of formaldehyde to propionaldehyde to diethyl amine was 1.1:1.0:1.0, amount of Mim]Ac was 10.0% (relative to propionaldehyde), Mannich reaction temperature was 45 ℃, reaction time was 50 min, decomposition temperature was 75 ℃, the yield of methacrolein was 95.3%. The structure of methacrolein was confirmed by 1H NMR. A preliminary study was carried out on the Mannich reaction mechanism catalyzed by Mim]Ac.
Keywords:ionic liquid  methacrolein  Mannich reaction
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