摘要
以4-氨基邻苯二甲酰亚胺和马来酸酐为原料,分别采用两步法和一步法合成了4-马来酰亚胺基取代邻苯二甲酰亚胺,探索了两种合成方法的最佳工艺条件,并通过红外光谱(FT-IR)、核磁共振氢谱(~1 H-NMR)对中间产物和目标产物进行了结构表征。分别采用两步法和一步法合成了4-马来酰亚胺基取代邻苯二甲酰亚胺,并对两种合成方法的工艺条件进行了优化。实验结果表明:采用一步法合成4-马来酰亚胺基取代邻苯二甲酰亚胺的最佳工艺条件为:甲苯与N,N-二甲基甲酰胺(DMF)为共溶剂的体积配比为1∶1,4-氨基邻苯二甲酰亚胺用量0.005mol,马来酸酐用量0.006mol,快速加热到120℃下反应,制得的4-马来酰亚胺基取代邻苯二甲酰亚胺的产率可达60.3%。由于一步法可对反应溶剂甲苯进行回收,相比两步法生产成本低。
4-maleimide substituted phthalimide was synthesized by two-step method and one-step method,using4-amino-phthalimide and maleic anhydride as the raw material.The best process conditions of two methods were studied,and the molecular structures of intermediate and target products were characterized by FT-IR and -1 H-NMR.The results indicated that,the best process conditions for the synthesis of 4-maleimide substituted phthalimide by onestep method were as follows：when using the mixture of toluene and DMF as reaction agent with the volume ratio was1∶1,the amount of 4-amino-phthalimide was 0.005 mol,the amount of maleic anhydride was 0.006 mol,and the temperature went up to 120℃ quickly,the product yield of prepared 4-maleimide substituted phthalimide was 60.3%.The one-step method had lower cost compared with two-step method,since the reaction agent of toluene can be recovered.
出处
《化工新型材料》
CAS
CSCD
北大核心
2017年第12期164-167,共4页
New Chemical Materials
基金
广东普通高校青年创新人才项目(2015KQNCX168)
五邑大学青年基金项目(2015zk04)
五邑大学青年基金创新团队项目(2015td01)
