四(m-氯苯基)卟啉及其锰络合物的合成

论文编号:HG035  论文字数:15464,页数:36

摘    要
 卟啉(Porphyrins)是在卟吩(Porphin)外环上带有取代基的同系物和衍生物的总称，当其氮上两个氢质子被金属取代后即成金属卟啉( Metallo-porphyries)。它是一类在生命体内具有重要作用的化合物，许多生命现象都有卟啉及其配合物的参加。近年来，有关卟啉类化合物的合成、应用日益受到人们的观注。
 各国科学家对它们的研究更深入和活跃，了解这类化合物在生命过程中的作用，将有助于我们更好地开发和利用它们。所以卟啉及其金属配合物合成、结构和性质研究受到人们的重视。
 本文采用单因素条件实验法，探讨了一种金属卟啉——四（m-氯苯基）卟啉及其锰络合物的合成方法与反应条件。实验结果表明：（1）可以采用“两步法”合成四（m-氯苯基）卟啉锰，即首先需要合成四（m-氯苯基）卟啉，再与金属盐络合制得四（m-氯苯基）卟啉锰。（2）合成卟啉的适宜反应条件为：反应溶剂为丙酸；原料吡咯和m-氯苯甲醛的摩尔投料比为1.00:1.03；反应物吡咯的浓度为0.32mol.L-1；反应时间为45min；反应温度为溶剂回流温度。在该条件下反应得到的四（m-氯苯基）卟啉的收率可达18%以上。（3）合成四（m-氯苯基）卟啉锰的适宜反应条件为：反应的溶剂为DMF；四（m-氯苯基）卟啉与醋酸锰的摩尔投料比为1:8；反应物四（m-氯苯基）卟啉的浓度为0.0222mol.L-1；反应时间为4h；反应温度为溶剂回流温度。在该条件下反应得到的四（m-氯苯基）卟啉锰的收率达85%以上。
  
关键词：四（m-氯苯基）卟啉；四（m-氯苯基）卟啉锰；收率

Abstract
 Porphyrins is the porphine outer ring has the substituent group homolog and the derivative general terms, when in after its nitrogen two protons by metallation, namely becomes metalloporphyrins. Porphyrin plays an important role in the field of life science. Many biological phenomena are depend on porphyrins and its complexes. In recent years, synthesis and application of porphyrin has been payed increasing attention to.
 All over the world, mang scientists on their research it is very deeper and active. In our life process, if we could understand these compounds’ function, we will develop and use them better. Therefore, studies on the synthesis,structure and properties of porphyrin and metalloporphyrins have been regarded seriously.
 Based on single factor experiment method is used to explore the method and the reactive conditions of synthesis for a metalloporphyrin—tetra(m-chlorphenyl)- porphyrin manganese(TCPPMn). The experimental results show that: (1) The TCPPMn has been synthesized from 3-chlorbenzaldehyde, pyrrole and acetate manganese by two-step method. First, the tetra(3-chlorphenyl)porphyrin(TCPP) is synthesized from 3-chlorbenzaldehyde and pyrrole, then the TCPPMn is synthesized from TCPP and acetate manganese. (2) The reaction condition of synthesis for TCPP is as follows: the reactive solvent is propionic acid, the molar ratio of pyrrole and 3-chlorbenzaldehyde is 1.00:1.02, the concentration of pyrrole is 0.32mol.L-1, the reactive time is 45 min, the reactive temperature is the temperature of solvent refluxing. In the condition, the yield of TCPP is more than 18%. (3) The reaction conditions of synthesis for TCPPMn is as follows: the reaction solvent is DMF, the molar ratio of TCPP and acetate manganese is 1:8, the concentration of TCPP is 0.0222mol.L-1; the reactive time is 4h, the reactive temperature is the temperature of solvent refluxing. Under the conditions, the yield of TCPPMn is more than 85%.
 
 Keywords: Tetra(m-chlorphenyl)porphyrin; Tetra(m-chlorphenyl)porphyrin Manganese ;  Yield
 
目    录
摘    要 I
Abstract II
第1章 引言 1
1.1 卟啉及金属卟啉概况 1
1.1.1 卟啉与金属卟啉的概述 1
1.2 卟啉及金属卟啉的合成工艺 2
1.2.1 卟啉及金属卟啉的传统的研究状况 2
1.2.2 合成卟啉及金属卟啉的新工艺研究 6
1.1.2 卟啉及金属卟啉化合物的应用研究 7
1.3本课题研究的目的和意义 10
1.4本文研究的主要内容 11
第2章 实验部分 12
2.1 实验试剂与药品 12
2.2 实验仪器与设备 12
2.3 反应原理 13
2.4 实验方法 13
2.4.1原材料预处理 13
2.4.2 实验操作步骤 14
2.4.3 分析与收率的计算 15
2.5工艺流程图 17
2.6反应装置图 18
第3章 实验结果与讨论 20
3.1 实验方案的设计 20
3.2合成四（m-氯苯基）卟啉的实验结果与讨论 21
3.2.1反应时间对产品收率的影响 21
3.2.2反应物吡咯的浓度对四（m-氯苯基）卟啉收率的影响 22
3.2.3 投料比对四（m-氯苯基）卟啉收率的影响 23
3.3合成四（m-氯苯基）卟啉锰的实验结果与讨论 24
3.3.1 投料比对四（m-氯苯基）卟啉锰收率的影响 24
3.3.2反应物卟啉的浓度对四（m-氯苯基）卟啉锰收率的影响 25
3.3.3反应时间对产品收率的影响 26
3.4 验证实验 26
第4章 结论 28
参考文献 29
致 谢 31

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