摘要
为开发一种绿色环保和操作简单的NCAs合成方法,以碳酸二甲酯(DMC)代替光气“一锅法”合成NCAs,研究反应过程中不同组分对产物的影响;利用变温FT-IR和TG-MS-IR技术研究中间体在催化剂表面的吸附和转变,最后中间体精准关环;解析DMC法精确合成NCAs的调控机制,并提供可能的反应催化机理。结果表明:当丙氨酸与DMC比例为1∶3、温度为150℃、反应9 h后,在DMF溶液中“一锅法”合成N-羧基丙氨酸酸酐产率最大为53.2%。
In order to develop a green and simple method to synthesize NCAs, dimethyl carbonate(DMC) was used to synthesize NCAs instead of phosgene by the "one-pot method". The influence of components on the product was studied, the modes of substrate adsorption and transformation over catalysts were characterized by variable-temperature FTIR and TG-MS-IR, the regulation mechanism of NCAs was precisely synthesized by DMC, and the possible catalytic mechanism was provided. It is shown that when the ratio of alanine to DMC was equal to 1∶3 and the reaction was carried out at 150 ℃ for 9 h in DMF, the highest yield of 53.2% for N-carboxy alanine anhydride(Ala-NCA)by the "one-pot method" was obtained.
作者
李振环
贾晓燕
LI Zhen-huan;JIA Xiao-yan(School of Material Science and Chemistry Engineering,Tiangong University,Tianjin 300387,China;State Key Laboratory of Separation Membranes and Membrane Processes,Tiangong University,Tianjin 300387,China)
出处
《天津工业大学学报》
CAS
北大核心
2021年第4期67-72,共6页
Journal of Tiangong University
基金
国家自然科学基金资助项目(21676202,21376177)。