木质素磺酸催化Biginelli反应合成3,4-二氢嘧啶-2(1H)-酮化合物  

Synthesis of 3,4-Dihydropyrimidin-2(1H)-one Compounds by Lignosulfonic Acid-Catalyzed Biginelli Reaction

作　　者：刘瑞岐 胡旭颖 毛渊渊 陈春霞[1] 彭进松[1] LIU Ruiqi;HU Xuying;MAO Yuanyuan;CHEN Chunxia;PENG Jinsong(College of Chemistry Chemical Engineering and Resource Utilization,Northeast Forestry University,Harbin 150040,China)

机构地区：[1]东北林业大学化学化工与资源利用学院,黑龙江哈尔滨150040

出　　处：《化学与粘合》2024年第2期107-112,116,共7页Chemistry and Adhesion

基　　金：黑龙江省自然科学基金(编号:LH2022B003);东北林业大学碳中和专项科学基金项目(编号:HKF221700013)。

摘　　要：为了绿色、高效地制备3,4-二氢嘧啶-2-酮衍生物,在无溶剂70℃条件下,以木质素磺酸为催化剂,单或多取代苯甲醛、尿素或硫脲与乙酰乙酸乙酯为原料,通过Biginelli反应“一锅法”合成了一系列3,4-二氢嘧啶-2(1H)-酮产物。产物结构经~1H和^(13)C NMR表征。研究结果表明:与经典的Biginelli反应条件相比,该催化体系对官能团普适性良好、产率优良,最高产率可达94%。该方法是一种具有绿色、温和、合成操作简单、产物纯化后处理方便等优点的制备3,4-二氢嘧啶-2-酮衍生物的新方法。In order to prepare 3,4-dihydropyrimidin-2-one derivatives in a green and efficient manner,a series of 3,4-dihydropyrimidin-2(1H)-one products are synthesized by the one-pot method via the Biginelli reaction at 70 ℃ in a solvent-free mode with lignosulfonic acid as catalyst,mono-or polysubstituted benzaldehyde,urea or thiourea and ethyl acetoacetate as raw materials.The structures of products are characterized with1H and13C NMR.The results show that the catalytic system is well adapted to the functional groups and gives excellent yields up to 94% compared with the classical Biginelli reaction conditions.A new method for the preparation of 3,4-dihydropyrimidin-2-one derivatives with the advantages of greenness,mildness,simple synthetic operation,and convenient treatment of the products after purification is developed.

关 键 词：木质素磺酸 BIGINELLI反应 无溶剂合成 3 4-二氢嘧啶-2(1H)-酮 

分 类 号：TQ426.92[化学工程] O641.4[理学—物理化学]