单 位：
安徽科技学院化学与材料工程学院;皖南医学院药学院
摘 要：
目的:优化N-甲基咪唑合成工艺。方法:以乙二醛、甲胺、氨水、多聚甲醛为原料,"一锅法"合成N-甲基咪唑,对N-甲基咪唑转化率的影响因素-投料顺序、反应温度、反应时间等进行条件优化,通过N-甲基咪唑的标准折光率曲线法准确、快速检测反应过程中N-甲基咪唑含量。所得产品N-甲基咪唑分别用氢谱、碳谱以及气质联用GC-MS进行表征。结果:以当量的多聚甲醛、氨水、甲胺、乙二醛的投料顺序,反应温度为60℃,反应时间为4小时,N-甲基咪唑的转化率高达98%。通过减压蒸馏除水,共沸剂环己烷精制,最后减压蒸馏得到的产品N-甲基咪唑纯度可达到99.5%。结论:该合成工艺具有产品转化率高,污水处理量少,检测方法快速高效的优点,适合于大规模工业生产。
译 名：
Research on the Synthetic Technology of N-methylimidazole
作 者：
ZHANG Ping;TANG Lin;ZHANG Ting;SONG Chang-chun;College of Chemistry and Material Engineering,Anhui Science and Technology University;College of Pharmacy,Wannan Medical College;
关键词：
N-methy-limidazole;;One-pot reaction;;Refractive inde
摘 要：
Objective: Different influential factors were optimized during the synthetic technology of N-methylimidazole in synthesizing process. Method: N-methy-limidazole was synthesized by a one-pot reaction with using glyoxal,methylamine,ammonia and paraformaldehyde as raw materials. The influential factor including materials adding order,reaction temperature and reaction time on the conversion rate of N-methy-limidazole were optimized. The content of N-methy-limidazole in synthesizing process was also accurately and rapidly detected through the standard curve of refractive index for N-methy-limidazole. The chemical structure of the final product was characterized by 1H and 13 C NMR spectroscopy and( GC-MS) mass spectrometry. Result:The results show that the conversion of the reaction is over 98% using the materials adding order of paraformaldehyde,ammonia methylamine and glyoxal,reaction temperature of 60℃ and reaction time of 4 h. The water was removed under vacuum and then using cyclohexane as azeotrope,the product was finally obtained with a purity of99. 5%. Conclusion: The synthetic technology has the advantages of high conversion,low sewage treatment,rapid and efficient detection method,which will be suitable for the industrial production.
