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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (6): 588-594. 上一篇    下一篇

研究论文

meso-5,10,15,20-四（取代2-噻吩基）卟啉及其配合物的合成与表征

李忠芳;王素文;宋文生;邓会宁;王亚权;王宇新   

  1. 天津大学化学工程院;山东理工大学科技研究院;天津大学
  • 发布日期:2003-06-25

Synthesis and Characterization ofmeso -Tetrakis(substitutional-2- thienyl) porphyrins and Their Complexes

Li Zhongfang;Wang Suwen;Song Wensheng;Deng Huining;Wang Yaquan;Wang Yuxin   

  1. School of Chemical Engineering and Technology,Tianjin University;Research Center of Science & Technology,Shandong University of Technology;State Key Laboratory of C1 Chemistry and Chemical Engineering,Tianjin
  • Published:2003-06-25

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用混合溶剂法合成了中位噻吩基取代的卟啉化合物：meso-四(2-噻吩基)卟啉 ，meso-四(4-溴-2-噻吩基)卟啉和meso-四(3-甲基-2-噻吩基)卟啉，产率达到36． 5％-39．3％，考察了溶剂的配比、反应温度、反应时间等因素对反应的影响，其 最佳反应条件为：溶剂配比：丙酸：乙酸：硝基苯：2：2(or3)：1；反应温度： 130~140t；反应时间：50-60min．研究了利用固相合成法合成上述卟啉化合物与过 渡金属盐形成配合物的配位反应，在40℃利用固相合成法合成了卟啉化合物与 Fe2'' Fe~3+，CO~2+，Ni~2+，Mn~2+等过渡金属离子形成的配合物，产率为81．1 ％~87．6％．利用元素分析，UV-vis，m，'HNMR， HRMS对卟啉化合物及其配合物 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．

关键词: 卟啉;噻吩 P;元素分析;紫外分光光度法;质子磁共振谱法;顺磁共振, 热稳定性;铁络合物;钴络合物;镍络合物;锰络合物

Three porphyrins, meso-5,10,15, 20-tetrakis(2-thienyl) porphyrin and meso-5, 10,15,2Q-tetrakis(4-bromo-2-thienyl)porphyrin and meso-5, 10,15)20-tetrakis(3-methyl-2-thienyl)poiphyrin, were synthesized in 35% ~ 39 % yields in a mixture solvent [ propionic acid: acetic acid: nitrobenzene = 2:2(or3) = l] at 130 ~ 140 t for 40 ~ 60 min from condensation of substitutional-2-thienyl aldehyde with pyrrole. 15 complexes of title porphyrins with Fe~(2+) , Fe~(3+) , Co~(2+) , Ni~ (2+) , Mn~(2+) were synthesized by the method of solid state synthesis at 40 °C in 81% ~ 87% yields. They were characterized by elemental analysis, UV-vis, ffi, 1H NMR, HRMS spectra. Their thermal decomposition characters were determined by TG-DTA, Showing 4 molecules of water is contained. The complexes decompose in two steps at 349 ~ 621 °C . Their magnetisms were characterized by EPR, all of tide porphyrins and their complexes have paramagnetism.

Key words: PORPHYRIN;THIOPHENE P;ELEMENTAL ANALYSIS;UV;1HNMR;PR;THERMAL STABILITY, IRON COMPLEX;COBALT COMPLEX;NICKEL COMPLEX;MANGANESE COMPLEX

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