二茂铁胺类衍生物和二茂铁双甲酸配合物的合成及电化学性质研究
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摘要
在本论文中，合成了两个新的二茂铁酰胺化合物7a和7b，通过元素分析，红外及核磁共振氢谱确定了化合物的组成和成份，进一步研究了新化合物的电化学性质；另外得到了两个含有二茂铁双甲酸的配合物单晶，确定了配合物的晶体结构，并对其进行了电化学性质研究。
第一部分
1．化合物的合成
(1)合成了两个新型二茂铁酰胺化合物7a和7b，通过IR、~1H NMR和元素分析等测试手段确证了化合物的结构。
合成路线如Scheme 1-1所示：
2．电化学性质研究
为了进一步研究二茂铁衍生物的性质，我们对六种二茂铁希夫碱衍生物9(a～c)和10(a～c)进行了电化学测定和量子化学计算的对比研究。
用多种电化学方法研究了两个系列的二茂铁衍生物的电化学性质，测定了它们在电极上反应过程中的动力学参数。结果表明：这些衍生物在电极表面的反应均受扩散控制；当二茂铁与苯坏直接相连时，二茂铁基团作为氧化还原中心，性质基本没有改变，氧化还原式量电位因苯环上取代基位置的不同有所不同；苯环取代基位置的不同不明显影响二茂铁衍生物在电极表面的扩散系数，而对电极反应的速率常数有较大的影响。
3．量子化学计算
对二茂铁衍生物7b和10c进行了量子化学计算与分析，对化合物的前线轨道成份、能量和净电荷进行了分析讨论。
第二部分
1．合成了两个含有二茂铁双甲酸的配合物A和B。
2．所得配合物均经过IR、~1H NMR和元素分析等鉴定手段进行了结构确证，并进行了电化学性质研究和红外光谱分析。
3．得到了配合物的晶体，并分析了它们的晶体结构，其中配合物A为二维的锯齿状聚合物，配合物B为双核的环状配合物。
In this thesis, two novel amino ferrocene derivatives 7a and 7b were synthesized and characterized by elemental analysis, IR and ~1H NMR spectra. The electrochemical properties of compounds were studied farther. In addition, two single crystals of the complexes containing 1.1'-ferrocenedicarboxylic were gained and the electrochemical properties of compounds were also studied.
Part 1
1. Synthesis of the compounds
Two novel compounds 7a and 7b of ferrocene derivatives were synthesized. The structure of the compounds was determined by element analysis, IR and ~1H NMR spectrum.
The synthesis of compounds was set out in Scheme1-1
2. Electrochemical properties of the compounds
In order to study the properties of the compounds deeply, six ferroenyl schiff bases derivatives 9(a~c) and 10(a~c) were also synthesized and studied by electrochemical properties and quantum calculation.
The electrochemical properties of twe series of the compounds were investigated by many electrochemical methods and determined kinetic parameters. The results indicated that: the reaction on the electrode were controlled by diffusion; the redox properties of ferrocene are not changed after connected with benzene, but it would be influenced by the different substitutions on the phenyl ring; the different substitutions on the phenyl ring is not obviously influence the diffusivities of the electrode reaction, but it has visible infection to constant of electrode action.
3. Quantum calculation of the compounds
The quantum calculation of these compounds were determined and described. We studied the components and proportions of molecular orbital energy and mulligan charges.
Part 2
1. Two complexes containing 1.T-ferrocenedicarboxylic A and B were synthesized,
2. All the complexes were characterized by elemental analysis and IR spectra. The electrochemical properties of the complexes were studied too.
3. Two single crystals of the complexes containing 1.1 '-ferrocenedicarboxylic were obtained, the X-ray single crystal structure analysis indicated that: the complex A is a polmer with two-dimensional constructure and the B is a binuclear cores complex.
第一部分
1．化合物的合成
(1)合成了两个新型二茂铁酰胺化合物7a和7b，通过IR、~1H NMR和元素分析等测试手段确证了化合物的结构。
合成路线如Scheme 1-1所示：
2．电化学性质研究
为了进一步研究二茂铁衍生物的性质，我们对六种二茂铁希夫碱衍生物9(a～c)和10(a～c)进行了电化学测定和量子化学计算的对比研究。
用多种电化学方法研究了两个系列的二茂铁衍生物的电化学性质，测定了它们在电极上反应过程中的动力学参数。结果表明：这些衍生物在电极表面的反应均受扩散控制；当二茂铁与苯坏直接相连时，二茂铁基团作为氧化还原中心，性质基本没有改变，氧化还原式量电位因苯环上取代基位置的不同有所不同；苯环取代基位置的不同不明显影响二茂铁衍生物在电极表面的扩散系数，而对电极反应的速率常数有较大的影响。
3．量子化学计算
对二茂铁衍生物7b和10c进行了量子化学计算与分析，对化合物的前线轨道成份、能量和净电荷进行了分析讨论。
第二部分
1．合成了两个含有二茂铁双甲酸的配合物A和B。
2．所得配合物均经过IR、~1H NMR和元素分析等鉴定手段进行了结构确证，并进行了电化学性质研究和红外光谱分析。
3．得到了配合物的晶体，并分析了它们的晶体结构，其中配合物A为二维的锯齿状聚合物，配合物B为双核的环状配合物。
In this thesis, two novel amino ferrocene derivatives 7a and 7b were synthesized and characterized by elemental analysis, IR and ~1H NMR spectra. The electrochemical properties of compounds were studied farther. In addition, two single crystals of the complexes containing 1.1'-ferrocenedicarboxylic were gained and the electrochemical properties of compounds were also studied.
Part 1
1. Synthesis of the compounds
Two novel compounds 7a and 7b of ferrocene derivatives were synthesized. The structure of the compounds was determined by element analysis, IR and ~1H NMR spectrum.
The synthesis of compounds was set out in Scheme1-1
2. Electrochemical properties of the compounds
In order to study the properties of the compounds deeply, six ferroenyl schiff bases derivatives 9(a~c) and 10(a~c) were also synthesized and studied by electrochemical properties and quantum calculation.
The electrochemical properties of twe series of the compounds were investigated by many electrochemical methods and determined kinetic parameters. The results indicated that: the reaction on the electrode were controlled by diffusion; the redox properties of ferrocene are not changed after connected with benzene, but it would be influenced by the different substitutions on the phenyl ring; the different substitutions on the phenyl ring is not obviously influence the diffusivities of the electrode reaction, but it has visible infection to constant of electrode action.
3. Quantum calculation of the compounds
The quantum calculation of these compounds were determined and described. We studied the components and proportions of molecular orbital energy and mulligan charges.
Part 2
1. Two complexes containing 1.T-ferrocenedicarboxylic A and B were synthesized,
2. All the complexes were characterized by elemental analysis and IR spectra. The electrochemical properties of the complexes were studied too.
3. Two single crystals of the complexes containing 1.1 '-ferrocenedicarboxylic were obtained, the X-ray single crystal structure analysis indicated that: the complex A is a polmer with two-dimensional constructure and the B is a binuclear cores complex.
引文
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