次卟啉制备新方法及其金属配合物的合成  

A New Approach to Prepare Deuteroporphyrin and Its Metallo-Complexes

作　　者：邓全知[1] 胡炳成[1] 孙呈郭[1] 徐士超[1] 刘祖亮[1] 

机构地区：[1]南京理工大学化工学院,南京210094

出　　处：《应用化学》2011年第11期1263-1268,共6页Chinese Journal of Applied Chemistry

基　　金：江苏省自然科学基金(BK2009386);南京理工大学科技发展基金(2010GJPY043)资助项目

摘　　要：研究了次氯化血红素在乙酸酐、氢溴酸体系中脱铁制备次卟啉的新方法。考察了反应时间、温度以及乙酸酐和氢溴酸与次氯化血红素的比例对反应产率的影响,讨论了其脱铁机理。实验结果表明,当次氯化血红素与氢溴酸和乙酸酐的摩尔比为1:6.3:61.2,温度为100℃,反应2 h时,脱铁产率高达96.3%。合成了一系列金属次卟啉配合物,考察了溶剂对卟啉配合金属难易程度及金属离子对卟啉S带和Q带的影响。用电喷雾串联质谱(ESI-MS-MS)、UV-Vis和IR表征了目标产物的结构。A facile demetalation of deuterohemin（DP） has been developed in a mixed solvent of acetic anhydride and hydrobromic acid.The influences of reaction time,bath temperature and the molar ratio on the yields were also investigated.Under the optimal reaction conditions for the demetalation of DP,the yield of 96.3% is obtained at the temperature of 100 ℃ for 2 h with the molar ratio of DP,hydrobromic acid and acetic anhydride about 1∶6.3∶61.2.A series of metallo-deuteroporphyrins was prepared and characterized by electrospray ionization tandem mass spectrometry（ESI-MS-MS）,UV-Vis and IR.In addition,we also studied the effects of different solvents on the synthesis of metalloporphyrins,and the properties of metal cations on the shift of S and Q bands of porphyrin.

关 键 词：次卟啉 次氯化血红素 合成 金属次卟啉 

分 类 号：O621[理学—有机化学]