N-异冰片基丙烯酰胺的合成  

Synthesis of N-isobornyl acrylamide

作　　者：周新成 陶钰 张成龙 徐徐[1,3] 杨益琴 王石发[1,3] ZHOU Xincheng;TAO Yu;ZHANG Chenglong;XU Xu;YANG Yiqin;WANG Shifa(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,Jiangsu,China;College of Light Industry and Food,Nanjing Forestry,University,Nanjing 210037,Jiangsu,China;Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources,Nanjing Forestry University,Nanjing 210037,Jiangsu,China)

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]南京林业大学轻工与食品学院,江苏南京210037 [3]南京林业大学林业资源高效加工利用协同创新中心,江苏南京210037

出　　处：《精细化工》2020年第4期860-864,共5页Fine Chemicals

基　　金：国家重点研发计划项目(2018YFD0600402)。

摘　　要：以丙烯腈和天然可再生资源莰烯为原料,在无溶剂条件下催化合成了N-异冰片基丙烯酰胺(NIBAM)。探索了催化剂种类及用量、物料配比、反应温度、反应时间对反应选择性和NIBAM得率的影响。采用正交实验确定了适宜的合成工艺条件:以FeCl3为催化剂,含量为10%(以莰烯、丙烯腈和水的总质量计,下同),n(莰烯)∶n(丙烯腈)∶n(水)=1∶3∶1,反应温度120℃,反应时间12 h。在此条件下,NIBAM选择性和得率分别为97.6%和90.3%。此外,采用HRMS、FTIR和NMR等分析技术对产物结构进行了确证。N-isobornyl acrylamide(NIBAM) was synthesized from acrylonitrile and natural renewable resource camphene under solvent-free conditions. Effects of the types and the dosages of catalysts, molar ratio of camphene to acrylonitrile and water, reaction temperature and reaction time on the reaction selectivity and the yield of NIBAM were investigated, and the optimum reaction conditions were determined by orthogonal tests as follows: the molar ratio of camphene to acrylonitrile and water was 1∶3∶1;FeCl3 was adopted as the catalyst, and the mass fraction of Fe Cl3 was 10%(based on total of acrylonitrile, camphene and water quality, the same below);reaction temperature 120 ℃, reaction time 12 h. The reaction electivity and the average yield of NIBAM under the aforesaid conditions were 90.3% and 97.6%, respectively. The structure of NIBAM was determined by HRMS, FTIR and NMR.

关 键 词：N-异冰片基丙烯酰胺 莰烯 丙烯腈 精细化工中间体 

分 类 号：TQ236[化学工程—有机化工]