2，6-二甲基吗啉及其衍生物的合成和工艺研究

【作者】 季世春；

【导师】 吕春绪； 李斌栋；

【作者基本信息】 南京理工大学 ， 应用化学， 2008， 硕士

【摘要】 2,6-二甲基吗啉是一种重要的农药和医药中间体,本文以浓硫酸为催化剂和溶剂,由二异丙醇胺在低温和高温两种不同的环境下环化脱水制备2,6-二甲基吗啉,并研究其最优条件,获得最好的产率88.59%。同时,利用精馏柱来研究其顺反-2,6-二甲基吗啉以及水的分离工艺,获得纯度99%以上的顺式-2,6-二甲基吗啉和反式-2,6-二甲基吗啉。接着,我们对反式-2,6-二甲基吗啉的异构化进行了研究,采用不同的复合金属为催化剂,将反式-2,6-二甲基吗啉在最优化的条件下转化为顺式-2,6-二甲基吗啉,其最优的产率达到50%,选择性达到了90%。另外,本文也完成了2,6-二甲基吗啉的下游产品顺式-2,6-二甲基-4-异十三烷基吗啉的合成路线。采用顺式-2,6-二甲基吗啉,在碳酸钠为碱性催化剂的条件下,和溴代异十三烷在110℃脱溴化氢获得,产率可以达到79.32%。更多还原

【Abstract】 2, 6-dimethyl-morpholine is very important mesial Substance of curative and safeguard reagent of agriculture. In this paper ,with diisopropanolamine containing from 0 to 20 of water for the raw material, 2, 6-dimethyl-morpholine could be synthesized with the overall yield of 88.59%. The reaction conditions were reaction at different temperatures （high temperature and low temperature）, concentrated sulfuric acid as the catalyst and solvent. At the same time, we researched the arts and crafts of separate cis-2, 6-dimethyl- morpholine, tran-2, 6-dimethyl-morpholine and water used by rectification, obtaining cis-2,6-dimethyl-morpholine and tran-2, 6-dimethyl-morpholine with 99% pureness. continuity, we also researched the isomerization of cis-2, 6-dimethyl- morpholine, cis-2, 6-dimethyl- morpholine was manufactured by catalytic isomerization of tran-2, 6-dimethyl-morpholine at the optimum condition with different metal complex as catalyst. The optimum yield could reach 50% and best selectivity also could reach 90%.In addition, we were also seeing about the preparation route of the downriver product of 2, 6-dimethyl-morpholine.With 2, 6-dimethyl-morpholine and 1-bromo- isotridecane as raw material ,2, 6-dimethyl-4-isotridecyl-morpholine was produced at 110℃temperature,Na₂CO₃ as the catalyst. The yield could reach 79.32%.更多还原