中间体DMAPAA合成工艺路线探索

Exploration Research on the Synthesis Processes of Intermediate DMAPAA

二甲氨基丙基丙烯酰胺(DMAPAA)是一种用于合成新型阳离子单体的关键中间体。本文拟在文献基础上以合成工艺、环保和安全条件等因素为指标,经论证分析和排序筛选出一类DMAPAA的合成工艺方法;进而,以操作方式和产物收率为主要指标,再选取3条合成路线,同步进行实验验证和排序;最后,先选择对其中一条工艺路线的影响因素进行了初步实验探索。结果表明,初步探索较佳条件下迈克尔加成收率为93.61%,酰胺化收率为95.78%,热裂解收率为62.35%,工艺总收率51.05%。通过上述研究,得到若干个可进一步探索的工艺方法和路线及其优化的参数范围,为后续DMAPAA合成路线选择、工艺优化、产物收率提高和季铵化研究奠定了一定的实验基础。

Dimethylamino propyl acrylamide(DMAPAA)is a key intermediate for the synthesis of novel cationic monomer.In this paper,on the basis of the literature,using the synthesis process,environmental protection and safety conditions as criteria firstly,a sort of DMAPAA synthesis process methods were selected through systemic analysis;Furthermore,using the operation mode and product yield as main indexes,three synthetic routes were selected for experimental verification,through comparing seven routes.Finally,serial exploration experiments concerning the effect of single processing factors on the yields of both intermediates and product were optimized.The results showed that the Michael addition yield was 93.61%,the amidation yield was 95.78%,the pyrolysis yield was 62.35%,and the total yield of the process was 51.05%under the optimal conditions.The study above has laid furtherly a valuable foundation of the investigating the synthesis route selection,process optimization,product yield improvement of DMAPAA and its quaternarization.