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作 者:朱秋迪 李磊 张奔 刘心韵 ZHU Qiudi;LI Lei;ZHANG Ben;LIU Xinyun(Key Laboratory of Functional Materials Chemistry of Guizhou Province,School of Chemistry and Materials Science,Guizhou Normal University,Guiyang 550001,China;School of Pharmaceutical Sciences,Guizhou Medical University,Guiyang 550025,China)
机构地区:[1]贵州师范大学化学与材料科学学院贵州省功能材料化学重点实验室,贵州贵阳550001 [2]贵州医科大学药学院,贵州贵阳550025
出 处:《合成化学》2023年第9期689-695,共7页Chinese Journal of Synthetic Chemistry
基 金:贵州省基础研究(自然科学)计划项目黔科合基础[2020]1Y030。
摘 要:喹喔啉及其衍生物是一种重要的化工中间体,被广泛用于生物医药领域,成为药物开发的一个新亮点。以壳聚糖为原料负载单质碘,使用浸渍法制备了壳聚糖负载单质碘(CS/I2)催化剂。通过傅里叶变换红外光谱(FT-IR)、X-射线衍射(XRD)、扫描电子显微镜(SEM)以及X-射线能量色散谱(EDS)对催化剂结构进行表征。以二苯基乙二酮与邻苯二胺缩合反应为模板反应,考察了反应时间、温度、溶剂、原料物质的量比和催化剂用量等因素对产物收率的影响。实验结果表明:碘单质成功负载于壳聚糖载体上,表现出良好的催化活性和较好的稳定性,模板反应产率为99.7%。反应扩大至克级时,产率可达97.3%。反应体系适用性良好,合成的10种喹喔啉衍生物产率为58.4%~99.7%。Quinoxaline and its derivatives are important chemical intermediates,which are widely used in the field of biomedicine to rise as a new bright spot in drug development.Chitosan supported iodine(CS/I2)catalyst was prepared by impregnation method.The structure of the catalyst was characterized by Fourier transform infrared spectroscopy(FT-IR),X-ray diffraction(XRD),scanning electron microscopy(SEM)and X-ray energy dispersion spectrometry(EDS).The effects of reaction time,temperature,solvent,molar ratio of raw materials and the amount of catalyst on the yield of the product were investigated.The experimental results showed that iodine was successfully loaded on the chitosan carrier and showed good catalytic activity and stability.The yield of template reaction was 99.7%.The yield of 97.3%was also obtained when the reaction was enlarged to gram.The reaction system has good applicability.The yields of 10 quinoxaline derivatives are 58.4%~99.7%.
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