| 过渡金属离子为模板的卟啉过渡金属配合物的合成研究 |
| Metal Ion as Template Use Synthesis of Metalloporphyrin Complexes |
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| 摘要: 系统研究了以过渡金属离子为模板的卟啉配合物的合成方法,探讨了金属离子加入的时间、加入方式,溶剂各组分配比,反应温度,反应时间等因素对反应的影响,得到最佳工艺参数:金属盐的加入最好在加入芳香醛和吡咯10～15min后,反应混合液的温度降到90℃以下,加入醋酸盐;混合溶剂配比为(2～5)∶(1～4)∶1;反应温度为120～145℃;反应时间为40～80min。并且利用该方法合成了34种金属卟啉配合物。利用元素分析,UV-Vis,IR, 1H NMR对金属卟啉配合物的结构进行了表征,利用TG-DTA研究了它们的热稳定性,利用EPR研究了它们的顺磁性。结果表明:该方法操作简便,产物易于分离、提纯,产率由原来两步合成法的10%～25%提高到35.1%～48%。 |
| 关键词: 模板反应 金属卟啉配合物 合成 表征 |
| 基金项目: |
| Abstract: 34 metalloporphyrin complexes were synthesized by one pot method of mixed solvents (propionic acid, acetic acid and nitrobenzene), using metal ion as template. The experimental results showed that the mixed solvents volume ratio is Vpropionic acid∶Vacetic acid∶Vnitrobenzene=(2～5)∶(1～4)∶1, at 120～145℃, the reactive time is 40～80min, the occasion of adding metal salt is: (1) After 10～15min of aromatic aldehyde and pyrrole were mixed; (2) Below 90℃ of mixture reactor; (3) Metal salt had better is acetate. The yields are 35.1%～48.0%. 34 metalloporphyrin complexes were obtained by this method. The complexes were characterized by elemental analysis, UV-Vis, IR, NMR. Their thermal decomposition characters were determined by TG-DTA, 4 molecules of water are contained in each complex molecule, and the decomposition of complexes occur in three steps between 353℃ and 605℃. Their magnetisms were characterized by EPR. The experimental result showed that this method of synthesis metalloporphyrin complexes is easy for operation and the products are easy separate and purify from reactive solu-tion. It is a simple and practical method for synthesis metalloporphyrin complexes. |
| Keywords: template reaction metalloporphyrin complex synthesis characterization |
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| 李忠芳,王素文,王纪孝,王亚权,王宇新.过渡金属离子为模板的卟啉过渡金属配合物的合成研究[J].无机化学学报,2003,19(7):691-698. |
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