N-(1-环己烯基)吗啉制备实验的改进

实验教材上以吗啉和环己酮为原料,对甲基苯磺酸为催化剂,甲苯作带水剂,通过缩合反应制备N-(1-环己烯基)吗啉。实验存在着耗时长、易造成实验室内有毒气体甲苯含量高、产品色泽深和收率低(小于60%)等不足。依据实验的目的、原理、内容不变的原则,采用n吗啉/n环己酮为1.6,预缩合反应1 h后加入共沸剂,反应加入对苯二酚,环己烷作共沸剂,分馏提纯产品等措施进行改进实验。改进后的实验,反应时间缩短了1 h、室内空气环境友好、产品近乎无色、收率可达80%以上。

The Improved Experimental Method to Synthesize N-(1-Cyclohexenyl)morpholine

The synthesis of N-(1-cyclohexenyl)morpholine in textbook is to use morpholine and cyclohexanone condensation reaction,p-toluene sulfonic acid as catalyst and toluene as water-carrying agent.There are some disadvantages of this method including long reaction time,high toluene content of toxic gas in laboratory,deep color of the product and low yield(<60%).Based on the same experimental purpose,principle and content,we propose some new operations as following to improve the experimental results:using morpholine and cyclohexanone(1.6 in mol ratio),pre-condensation reaction of 1 h before adding water carrying agent,adding hydroquinone into system,using cyclohexane as water carrying agent and fractionating to purify the product.The improved experiment shows that the reaction time is shortened by 1 h,the indoor air environment is friendly,the product is almost colorless,and the yield could reach more than 80%.