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作 者:何顺莉[1] 罗玉兰[1] 宋文婷[1] 余光勤[1] 吴庆[1] 袁泽利[1]
出 处:《化学世界》2016年第2期78-82,共5页Chemical World
基 金:国家基金资助项目(81360471);贵州省科学技术基金项目(黔科合J字2011[032];国地方高校国家级及贵州省教育厅大学生创新实验项目(201310661001)
摘 要:利用壳聚糖的轴向配位作用固定化杂大环Cu(Ⅱ)配合物,并利用红外光谱(FT IR)和扫描电镜(SEM)等现代分析手段对其进行了结构和组成表征。对关键中间体L进行了常规合成法和微波合成法考察。结果表明:微波法具有操作简单、反应时间短、条件温和、产率高及副反应少等优点,并探讨了微波合成法合成杂大环中间体L的最佳合成条件:以甲醇做溶剂,在m(二乙撑三胺)∶m(2,2′-(乙基氧)-双苯甲醛)为1∶1、微波功率为400 W、60℃下微波反应0.5h。并在模拟生理条件(pH=7.40,37℃)下,利用Gress试剂法考察了目标配合物催化S-亚硝基硫醇释放NO性能。结果表明:目标配合物具有稳定催化释放一氧化氮性能。The complex of chitosan-Cu( II )- hetero-macrocycle has been synthesized relying on the coordi- nativepotential of chitosan and characterized FT IR and SEM. The synthesis method were also compared with those of the sample prepared by traditional methods. The result showed that the process under micro- wave irradiation had many merits with excellent yield, short time, simple operation and less secondary reac- tion. The favorable reaction conditions of preparing the middle macrocyclic compound(L) were found as follows: the reacting time was about 0.5 h, the reacting temperature was 60 ℃,400 W, and the mol ratio of 2,2'-(ethylenedioxy)bis -benzaldehyde to diethylenetriamine was 1 : 1, and the solvents were methanol under microwave irradiation. The NO release profiles for title complex in PBS solution (pH =7.4, 37℃ ) was investigated by the Griess assay. The results show that the title complex efficiently decompose S-Ni- trosothiols to NO catalytically.
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