非催化条件下绿色合成3,4-二氢嘧啶酮衍生物  

Green synthesis of 3,4-dihydropyrimidinones derivatives without catalyst

作　　者：宋志国 赵润秋 万鑫[2] 赵爽[2] 王敏[2] SONG Zhi-guo;ZHAO Run-qiu;WAN Xin;ZHAO Shuang;WANG Min(Experimental Center,Bohai University,Jinzhou 121013,China;College of Chemistry&Chemical Engineering,Bohai University,Jinzhou 121013,China)

机构地区：[1]渤海大学实验中心,辽宁锦州121013 [2]渤海大学化学化工学院,辽宁锦州121013

出　　处：《化学研究与应用》2020年第9期1596-1600,共5页Chemical Research and Application

基　　金：辽宁省自然科学基金项目(2019-MS-005)资助;辽宁省教育厅项目(LJ2019007,LQ2017010)资助;辽宁省博士启动基金项目(2019-BS-005)资助。

摘　　要：在无溶剂、无催化剂、70℃条件下,以等摩尔醛、乙酰乙酰苯胺和甲基脲为原料,通过三组分“一锅法”合成了一系列N 1-甲基取代的3,4-二氢嘧啶酮衍生物。考察了原料用量和反应温度对产率的影响,确定较佳的反应条件为:n醛∶n乙酰乙酰苯胺∶n甲基脲=1∶1∶1,反应温度为70℃。该方法的优点是反应条件温和、绿色,无需使用催化剂和溶剂。产物结构通过1H NMR、13 C NMR、IR和元素分析进行表征和确证。此外,对目标产物进行了固态荧光检测,证明其具有良好的荧光性质。Three components one-pot synthesis of N 1-methyl substituted 3,4-dihydropyrimidinones derivatives from equimolar aldehyde,acetoacetanilide and methyl urea without catalyst and solvent at 70℃was reported.The effects of the molar ratio of raw materials and the reaction temperature on the yields were investigated.The optimum reaction conditions were as follows:n(aldehyde)∶n(acetoacetanilide)∶n(methyl urea)=1∶1∶1,reaction temperature was 70℃.The advantages of the protocol were mild and green conditions,and no catalyst or solvent was needed.The structure of products were characterized by 1H NMR,13 C NMR,IR and elemental analysis.In addition,the good fluorescent properties of the target product was proved by the fluorescence detection in solid state.

关 键 词：BIGINELLI反应 无溶剂 无催化剂 绿色合成 

分 类 号：O626.4[理学—有机化学]