低共熔溶剂中2,5-二苯基噁唑的绿色合成研究  

Green Synthesis of 2,5-Diphenyloxazole in Deep Eutectic Solvents

作　　者：闫浩 田杨锴 周小强 胡梦 杨佳艺 李小蓉[1] YAN Hao;TIAN Yangkai;ZHOU Xiaoqiang;HU Meng;YANG Jiayi;LI Xiaorong(College of Pharmacy,Shaanxi University of Chinese Medicine,Xianyang Shaanxi 712046,China;College of Chinese Meteria Medica,Beijing University of Chinese Medicine,Beijing 102488,China;College of Chemistry and Materials,Weinan Normal University,Weinan Shaanxi 714099,China)

机构地区：[1]陕西中医药大学药学院,陕西咸阳712046 [2]北京中医药大学中药学院,北京102488 [3]渭南师范学院化学与材料学院,陕西渭南714099

出　　处：《当代化工》2024年第10期2298-2301,2308,共5页Contemporary Chemical Industry

基　　金：陕西省重点研发计划项目(项目编号:2023-YBSF-278);咸阳市重点研发计划项目(项目编号:L2022ZDYFSF054);中国博士后科学基金项目(项目编号:2021M690474);陕西省教育厅科研计划项目(项目编号:23JK0432);陕西中医药大学校级科研项目(项目编号:2020GP08)。

摘　　要：以低共熔溶剂为反应溶剂,采用苯甘氨酸与α-溴代苯乙酮为起始反应底物,在碘催化下完成了2,5-二苯基噁唑的绿色合成,通过1H NMR、13C NMR、MS对目标化合物的结构进行表征,并对该反应条件进行了方法学研究。得到2,5-二苯基噁唑合成的最佳反应条件如下:反应溶剂为氯化胆碱-草酸(物质的量比1∶2)低共熔溶剂,反应温度为120℃,反应时间为5 h,催化剂碘物质的量为0.03 mmol。在上述条件下,反应收率达到46%,且后处理操作简单,无需柱层析纯化,可重复性好。The green synthesis of 2,5-diphenyloxazole was accomplished by using a deep eutectic solvent as the reaction solvent,and using phenylglycine andα-bromoacetophenone as the starting reaction substrates catalyzed by iodine.The structure of the target compound was characterized by 1H NMR,13C NMR,and MS.Then the methodological study of reaction conditions was carried out.The optimal reaction conditions for the synthesis of 2,5-diphenyloxazole were obtained as follows:the reaction solvent choline chloride-oxalic acid(molar ratio 1∶2)was used as a deep eutectic solvent;the reaction temperature was 120℃;the reaction time was 5 h;the catalyst iodine dosage was 0.03 mmol.Under above conditions,the reaction yield could reach 46%.The reaction post-processing operation was simple,without the need for column chromatography purification,and the reaction had good reproducibility.

关 键 词：低共熔溶剂 苯甘氨酸 α-溴代苯乙酮 2 5-二苯基噁唑 绿色合成 

分 类 号：TQ201[化学工程—有机化工] O626.24[理学—有机化学]