4-酰基吡唑啉酮配合物的合成方法与结构

综述了4-酰基吡唑啉酮及其配合物的合成方法和结构特征,介绍了非水溶剂法、水相合成法、固相合成法等合成方法适用的体系。分析评价了4-酰基吡唑啉酮以烯醇双氧、共轭双酮氧参与中心离子包含主族金属元素、副族金属元素、稀土金属元素等配位成键,形成6配位、8配位、单核、双核和多核配合物的结构关系。     

缩苯胺希夫碱合铜配合物的合成和表征

酰基吡唑啉酮配合物由于在功能材料、金属离子萃取、生物活性等领域应用广泛,其新型配体及配合物的合成、性能及配体与中心离子间的作用成为配位化学研究的热点。实验在乙醇溶剂中进行反应,以1-苯基-3-甲基-4-庚酰基-吡唑啉酮-5为母体,进一步通过1-苯基-3-甲基-4-庚酰基-吡唑啉酮-5与苯胺反应合成了缩苯胺希夫碱,然后再用缩苯胺希夫碱与金属铜离子反应生成了缩苯胺希夫碱合铜配合物。最后通过红外光谱测定其官能团、紫外光谱测定其含量和荧光分析等各种表征手段来佐证其结构和组成。     

己酰基吡唑啉酮锌配合物的合成与表征

酰基吡唑啉酮配合物在功能材料、金属离子萃取、生物活性等领域应用广泛。以1-苯基-3-甲基-吡唑啉酮-5(PMP)为母体,设计合成出4-己酰基吡唑啉酮(HL),通过4-己酰基吡唑啉酮配体(HL),非水溶剂法与金属Zn盐成功合成金属配合物,应用光学和热学分析检测仪对HL与金属配合物进行性能表征。红外光谱中发现,烯醇羟基已去质子化发生配位,吡唑啉酮环共轭形成大的离域键。热重分析测试表明金属配合物在107℃时开始失去水分子,配合物存在并且应用环境不高于107℃。     

席夫碱-镍配合物的合成与表征

以1-苯基-3-甲基-4-己酰基-吡唑啉酮-5为母体,设计合成出4-己酰基吡唑啉酮缩苯胺席夫碱(HQ),通过非水溶剂法将4-己酰基吡唑啉酮缩苯胺席夫碱(HQ)与金属盐Ni反应成功合成金属配合物,应用光学检测仪对HQ与金属配合物进行性能表征。红外光谱中发现,在510cm-1处有O-Ni键生成,佐证配合物配位成功;在紫外光谱中,席夫碱-镍配合物的最强吸收波长出现在306nm处;通过荧光谱图可以找到金属配合物的最强激发波长是245nm,最强发射波长是349nm。实验数据为研究席夫碱在更多领域的实际应用提供了理论依据。     

取代苯基酰基吡唑啉酮Zn(Ⅱ)、Ni(Ⅱ)配合物的合成与表征

合成新型酰基吡唑啉酮化合物及其金属配合物,研究其热稳定性。在非水溶剂中,对硝基苯肼与乙酰乙酸乙酯反应制得酰基吡唑啉酮。通过回流新配体和金属醋酸盐合成了配合物。合成了新β-双酮试剂,1-对硝基苯基-3-甲基-4-(α-呋喃甲酰基)吡唑啉酮-5(HL)及其锌和镍的配合物。元素分析及摩尔电导值表明配合物的组成为[NiL2]·2C2H5OH·[ZnL2]·2C2H5OH。通过红外光谱、紫外光谱、差热—热重分析对配合物进行了表征。结果表明配合物的中心离子均为4配位。它们加热至185℃分解。     

新型过渡金属配合物的合成、表征及生物活性研究

为了寻找更好的生物活性化合物,以1-苯基-3-甲基-5-吡唑啉酮和苯甲酰氯为原料,二氧六环为溶剂,回流反应合成了4-酰基吡唑啉酮配体及4种过渡金属配合物,通过元素分析、红外光谱、差热-热重分析、紫外光谱等对其结构进行了表征,表明配合物组成分别为:Cu(L)2、Zn(L)2、Ni(L)2、Mn(L)2;同时利用抑菌圈大小...     

新型酰基吡唑啉酮钬(Ⅲ)、钕(Ⅲ)配合物的合成与表征

酰基吡唑啉酮配合物在分析化学、金属侵蚀、催化,生物,发光材料等领域具有广泛的应用。研究了酰基吡唑啉酮钬(Ⅲ)、钕(Ⅲ)配合物的各种性质。利用1-苯基-3-甲基-吡唑啉酮-5为母体设计合成出了1-苯基-3-甲基-4-己酰基吡唑啉酮-5(HL),再将HL与金属钬和钕的三价盐发生化合反应制备这两种金属的酰基吡唑啉酮配合物,并使用部分光学仪器对化合物进行表征。通过红外光谱分析发现钬(Ⅲ)配合物在476cm-1处有O-Ho键生成、钕(Ⅲ)配合物在469cm-1处有O-Nd键生成;通过差热-热重分析测试可以看出这两种配合物的分解温度较高;通过荧光性能测试得到钬(Ⅲ)配合物,钕(Ⅲ)配合物的最大激发波长和最大发射波长,且发现它们的荧光强度较大。     

新型酰基吡唑啉酮配合物的合成、表征及生物活性研究

以1-苯基-3-甲基-5-吡唑啉酮和苯甲酰氯为原料,二氧六环为溶剂,回流反应合成了4-酰基吡唑啉酮配体及4种过渡金属配合物,通过元素分析、红外光谱、差热一热重分析、紫外光谱等对其结构进行了表征,表明配合物组成分别为:Cu(L)2、Zn(L)2、Ni(L)2、Mn(L)2;同时利用抑菌圈大小对2种细菌和4种真菌进行了生物...     

对甲苯胺缩铜配合物的合成与表征

己酰基吡唑啉酮配合物在功能材料、金属离子萃取、催化,光电学,生物活性等领域应用广泛。以1-苯基-3-甲基-吡唑啉酮-5为母体设计合成了1-苯基-3-甲基-4-庚酰基吡唑啉酮-5(HL),通过HL制备出对甲苯胺席夫碱,将对甲苯胺席夫碱与乙酸铜合成出对甲苯胺缩铜配合物,并用光学仪器对其进行性能表征。通过紫外光谱发现了配体与金属配合时配体的共轭结构发生了变化,致使吸收光谱发生位移;在红外谱图中发现了配合物在570cm-1处有O-Cu键生成;通过荧光检测发现席夫碱和配合物在荧光谱图中均能找到激发波长和发射波长。     

萘乙酰基吡唑啉酮及其席夫碱的合成与表征

在非水溶剂中合成出一种未见报道的新型酰基吡唑啉酮试剂:1-苯基-3-甲基-4-萘乙酰基-吡唑啉酮-5(PMNAP)及其3 种席夫碱化合物.通过元素分析、红外光谱、质谱和核磁共振氢谱对其进行了结构表征.表征结果显示:PMNAP以酮式结构存在,形成席夫碱后的3种化合物均以酮式和烯醇式两种结构并存.     

分子氧氧化环己烯负载型催化剂的制备与选择

在乙醇溶剂中,合成出三种希夫碱配体和四种不同金属离子希夫碱配合物,并用红外线对其结构进行表征,表明合成出希夫碱配体及其配合物.接着以分子氧为氧源,金属希夫碱配合物为催化剂,考察其对环己烯的催化氧化性能,从而筛选出较佳的配位体:水杨醛缩乙二胺配位体和较佳的金属离子钴离子;进而以水杨醛缩乙二胺钴配合物为均相催化剂,采用两种方法将其负载在硅藻土、活性炭、分子筛和石英砂上,并考察该非均相催化剂催化活化分子氧氧化环己烯的催化氧化性能,结果表明,硅藻土为较佳无机载体,固载时,柔性配体法优于浸渍法.     

电有机合成3,5-二溴水杨醛缩丝氨酸过渡金属配合物的研究

研究了3,5-二溴水杨醛缩丝氨酸过渡金属配合物的绿色电化学合成工艺。以3,5-二溴水杨醛及丝氨酸为原料,无水乙醇为溶剂,合成3,5-二溴水杨醛缩丝氨酸席夫碱。以席夫碱为原料,分别以金属铜、镍、锌片等为阳极,铂片为阴极,乙腈为溶剂,季铵盐为电解质,通入直流电电解,获得了3,5-二溴水杨醛缩丝氨酸席夫碱铜(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)配合物,同时利用正交实验优化了配合物电化学合成工艺条件。利用红外光谱、紫外光谱、热分析等手段对过渡金属配合物进行结构表征,结果表明达到了预期的合成目的。     

The Synthesis and Characterization of New Schiff Bases and Investigating them in Solvent Extraction of Chromium and Copper

New Schiff bases containing nitrogen, sulfur and oxygen donor atoms, were designed and synthesized in a multi—step reaction sequence. The Schiff base(I) was used in solvent extraction of metal chlorides such as Cu(II) from aqueous phase to the organic phase. The influences of the parameter functions, such as pH, solvent, ionic strength of aqueous phase, aqueous to organic phase, and concentration of the extractant were investigated to shed light on their chemical extracting properties upon the extractability of metal ions. The effect of chloroform, dichloromethane, and nitrobenzene as organic solvents over the metal chlorides extraction was investigated at 25 ± 0.1°C by using flame atomic absorption and the result is that the ability of extraction in solvents as follows C₆H₅NO₂ > CHCl₃ > CH₂Cl₂.     

Rapid extraction of Cu(II) heavy metal from industrial waste water by using silver nanoparticles anchored with novel Schiff base

A new Schiff base named N-(4-hydroxy-3-methoxy benzylidine)-biphenyl-4-amine was synthesized from refluxing of equimolar quantity of vanillin and biphenyl-4-amine in alcoholic medium. Its composition, properties, and morphology were characterized by elemental analysis, FTIR (Fourier-transform infrared spectroscopy), UV–vis (ultraviolet visible spectroscopy), nuclear magnetic resonance spectroscopy, and mass spectral studies. Then, silver nanoparticles were synthesized by chemical reduction method and characterized by scanning electron microscope, UV–vis, FTIR, and mass spectra. The silver nanoparticles are then trapped with Schiff base by suitable method. The metal ion was analyzed by atomic absorption spectroscopy. Sugarcane bagasse (SCB) was used as solid phase for the removal of heavy metal from industrial waste water. Activation of solid phase was done with the base and acid, respectively. The Ag nano@Schiff base was adsorbed on the SCB. The effects of several parameters that affect the adsorption of Cu(II) metal ion including initial metal ion concentration, contact time, Schiff base weight, and pH were analyzed.     

Schiff Base Complexes in Macromolecules

Summary  Schiff base metal complexes are a class of compounds that have been studied extensively because of their attractive chemical and physical properties, and their wide-ranging applications in numerous scientific areas. Researchers have incorporated Schiff base complexes into polymers, generating new materials with useful mechanical, thermal, chemical, and electronic properties. This work comprehensively reviews the developments in macromolecules containing Schiff base metal complexes, emphasizing new synthetic strategies and characterization techniques that were used to prepare and study these polymers. This paper is dedicated to the pioneering research of Dr. Ian Manners.     

Schiff Base型大环化合物的合成研究进展

研究发现Schiff base型大环化合物具有优异的抗菌和过渡金属离子的萃取性能,已经成为有机化学的研究热点之一。综述了Schiff base型大环化合物的合成方法研究进展,并对合成中的一些诸如模板离子的大小与缩合比,脱模板作用等问题作了简要探讨。     

New antimicrobial agents: The synthesis of Schiff base polymers containing transition metals and their characterization and applications

A new polymeric Schiff base containing formaldehyde and 2‐thiobarbituric acid moieties was synthesized by the condensation of a monomeric Schiff base derived from 2‐hydroxyacetophenone and hydrazine. Polymer–metal complexes were also synthesized by the reaction of the polymeric Schiff base with Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) acetate. The polymeric Schiff base and its polymer–metal complexes were characterized with magnetic moment measurements, elemental analyses, and spectral techniques (infrared, ¹H‐NMR, and ultraviolet–visible). The thermal behaviors of these coordination polymers were studied by thermogravimetric analysis in a nitrogen atmosphere up to 800°C. The thermal data revealed that all of the polymer–metal complexes showed higher thermal stabilities than the polymeric Schiff base and also ascribed that the Cu(II) polymer–metal complex showed better heat resistant properties than the other polymer–metal complexes. The antimicrobial activity was screened with the agar well diffusion method against various selected microorganisms, and all of the polymer–metal complexes showed good antimicrobial activity. Among all of the complexes, the antimicrobial activity of the Cu(II) polymer–metal complex showed the highest zone of inhibition because of its higher stability constant and may be used in biomedical applications. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Chitosan Biopolymer Schiff Base: Preparation,Characterization, Optical,and Antibacterial Activity

Natural biopolymer used for hydrogels has attracted increasing attention in the multifaceted areas of biomedical science and engineering. The authors prepared chitosan biopolymer Schiff base by solvent exchange method using a simple aliphatic crosslinker, crotanaldehyde. The identity of Schiff base was confirmed by UV-vis and Fourier-transform infrared spectroscopy. The chitosan Schiff base was evaluated by XRD, TGA, DSC, and SEM. The microbiological screening results demonstrated the antibacterial activity of Schiff base against Escherichia coli and Staphylococcus aureus bacteria. These results suggest that the newly prepared Schiff base may open a new perspective in biomedical applications.     

牛磺酸配合物的合成与应用研究进展

牛磺酸具有广泛的生理药理作用,但是它作为一种配体与阳离子进行配位的报道却很少。从牛磺酸的配位化学角度出发,论述了牛磺酸金属配合物和牛磺酸席夫碱金属配合物的合成方法,并且对牛磺酸配合物的应用进展作了简要综述。