摘要
β-酮基丁酸酯和N-芳基取代的β-酮基丁酰胺通过双乙烯酮与ROH(R=烷基或芳基)或N-甲基苯胺的反应以及乙酰乙酸乙酯的芳胺解反应制备得到。两类化合物与2~3倍物质的量的芳香胺在无溶剂条件于室温下以质子酸为催化剂反应,以中高收率得到一系列的目标化合物,并对它们进行了1HNMR、13CNMR、IR和ESI-MS表征。其中两个还通过X-射线单晶衍射测定了其分子结构。实现了此类化合物无溶剂无金属催化条件下的简单合成。
Acetylacetic esters and N-aryl acetylacetamides were synthsized by the reaction of diketene with alcohols or N-methylaniline and by treatment of ethyl acetylacetate with arylamines,respectively.The title compounds were obtained in moderate to high yield by facial condensation of acetylacetic esters and N-aryl acethlacetamide with 2 ~ 3 folds of various arylamines catalyzed by concentrate protic acid at room temperature and in solvent-free condition.The samples were readily purified by recrystallization or by column chromatolography,and were confirmed by1 HNMR,13 CNMR,IR and ESI-MS.The crystal structures of two compounds were determined by X-ray single crystal diffraction analysis.A simple synthesis method of such compounds under solvent-free and metal-free catalysis was achieved.
作者
鲁赟
崔亮
孙志明
雷珺宇
义建军
肖勇
胥明亮
庄俊鹏
郝海军
LU Yun;CUI Liang;SUN Zhi-ming;LEI Jun-yu;YI Jian-jun;XIAO Yong;XU Ming-liang;ZHUANG Jun-peng;HAO Hai-jun(College of Science,Beijing University of Chemical Technology,Beijing 100029,China;Key Laboratory of Synthetic Resin,Petrochemical Research Institute,PetroChina Company Limited,Beijing 102206,China;Fushun Petrochemical Company,PetroChina Company Limited,Fushun 113008,China)
出处
《化学试剂》
CAS
北大核心
2019年第3期274-282,共9页
Chemical Reagents
基金
中国石油天然气股份有限公司石油化工研究院科研项目(PRIKY16018)