应用化学2025，Vol.42Issue(4)：533-541,9.DOI:10.19894/j.issn.1000-0518.240354
酸性低共熔溶剂中Biginelli反应的克级合成
Gram-Scale Biginelli Reaction in Acidic Deep Eutectic Solvent
摘要
Abstract
A rapid and efficient synthesis of 3,4-dihydropyrimidin-2(1H)-(thio)ones was achieved under solvent-free conditions using choline chloride/trifluoromethanesulfonic acid(ChCl/TfOH)deep eutectic solvent as a catalyst.The condensation reaction of benzaldehyde,ethyl acetoacetate,and urea was used as a template reaction to investigate the effects of the type and amount of deep eutectic solvent,temperature,and starting material ratio on the reaction.Results showed that the optimized conditions were as follows:benzaldehyde(5 mmol),ethyl acetoacetate(5 mmol),urea(7.5 mmol),ChCl/TfOH(2.5 mmol),80℃and 5 min.The yield of the target product was as high as 95%under the optimized conditions.The reaction system also showed good compatibility with different substrates,with product yields ranging from 82%to 95%.In addition,gram-scale synthesis could be realized for this reaction,and the yield was up to 87%after 15 min.The advantages of this system are fast reaction speed,high yields,and no need for further purification of the products.Moreover,the recovery of deep eutectic solvent could be achieved through simple extraction.关键词
Biginelli反应/二氢嘧啶-2(1H)-酮/硫酮/低共熔溶剂/绿色合成/克级合成Key words
Biginelli reaction/Dihydropyrimidin-2(1H)-(thio)one/Deep eutectic solvent/Green synthesis/Gram-scale synthesis分类
化学引用本文复制引用
王丹,王亮..酸性低共熔溶剂中Biginelli反应的克级合成[J].应用化学,2025,42(4):533-541,9.基金项目
江苏省第六期"333"高层次人才培养工程和常州工程职业技术学院校科研基金(Nos.11130300123003,11130900123001)资助 Supported by the"333"High-level Talent Project of Jiangsu Province and Research Fund of Changzhou Vocational Institute of Engineering(Nos.11130300123003,11130900123001) （Nos.11130300123003,11130900123001）
