酰基吡唑啉酮希夫碱及配合物的合成、结构及生物活性

综述了酰基吡唑啉酮希夫碱及配合物的合成、结构和生物活性.介绍了非水溶剂法、固相合成法、水相合成法、溶剂热合成法等配合物合成方法.分析了酰基吡唑啉酮希夫碱参与过渡金属、稀土金属配位成键的方式,以及相应配合物空间构型为四面体、平面正方形、八面体、十二面体的结构关系.讨论了标题化合物对金黄葡萄球菌、枯草杆菌、大肠杆菌等的抑制...     

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。     

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。     

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。     

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。     

酰基吡唑啉酮缩邻氯苯胺席夫碱Ni(Ⅱ)、Al(Ⅲ)配合物的合成与表征

酰基吡唑啉酮缩有机胺是新型席夫碱配体,对金属离子具有较好的萃取性能,具有一定的传递电子作用、光致发光作用及较强的抗菌抗病毒生物活性。为进一步拓宽酰基吡唑啉酮类配合物的研究领域,合成了1-苯基-3-甲基-4-(α-呋喃甲酰基)吡唑啉酮-5缩邻氯苯胺新型席夫碱试剂及其镍和铝配合物。元素分析、摩尔电导数据表明配合物的组成分别为:Ni(L)2.2H2O、Al(L)3.H2O。通过红外光谱、紫外光谱、差热-热重分析对配合物进行表征。     

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...     

丙二酸二乙酯的合成进展

丙二酸二乙酯是重要的有机合成中间体,广泛应用于医药、染料和香料等工业。传统的氰化钠法由于流程长,收率低,污染环境而亟待改进。近年来研究比较活跃的催化羰基化法,是典型的原子经济型反应,步骤少,收率高,绿色环保,与其它合成方法比较具有较大的优势,可望替代传统方法。     

酰基吡唑啉酮修饰玻碳电极对维生素C组分的电化学分析

制备了呋喃甲酰基吡唑啉酮修饰玻碳电极,通过循环伏安法用该电极对维生素C组分进行分析。考察了支持体系的pH值、配体修饰量、扫描起始电位、扫描速度等对电极反应的影响。实验结果表明,在NaH2PO4-Na2HPO(4pH=5.5)缓冲溶液中,测定体系于0.5V(vs.SCE)处出现一尖锐、灵敏的修饰吸附峰。其浓度线性形范围关系:Y=6.70137+19.9381XR=0.99833。采用标准加入法对实际样品进行了检测,结果满意。     

Solution phase synthesis of amyloid-cleaving catalysts, two [1,3,5]triazine based compounds

Solution phase synthetic method for amyloid-cleaving catalysts was developed, which bears triazine core, scaffold with bulky and that have various solubility properties; Co(III) complex of cyclen (1,4,7,10-tetraazacyclododecane) for catalytic group, and two imaging agents for binding group. This synthetic method was identified by H-NMR, C-NMR for intermediates and MS for the last products. The yields by this method surpassed solid phase synthesis and took much lower labor, expense, and time. The products which were synthesized by solution phase synthetic method showed good catalytic activities.     

The synthesis of water-soluble CDM-AM copolymer by irradiation and its solubilization effect on hydrophobic drugs

The β-cyclodextrin-acrylamide (CDM-AM) copolymer was prepared from acrylamide and β-CD maleate (CDM) using ⁶⁰Co γ-ray irradiation method. The optimized preparation conditions for the CDM-AM copolymer are as follows: CDM:AM mass ratio of 1:1; irradiation dose of 4 kGy; and using 20 mL of DMF water solution. The yield rate of CDM-AM was 75% in grams using these synthetic conditions. The effects of the CDM-AM copolymer on the solubility and fungicidal activity of natamycin (NM) and carbendazim (MBC) were investigated. The stability constant of NM·CDM-AM and MBC·CDM-AM complexes at 303 K were of 13,446.06 M^?1 and 2595.3 M^?1, respectively. The complexes were characterized using phase solubility diagrams, NMR spectra and FT-IR spectra. The analysis of the biological activities of these two complexes indicated that they possessed enhancing fungicidal activities compared to NM and MBC alone.     

Baeyer–Villiger oxidation of ketones with hydrogen peroxide catalyzed by cellulose-supported dendritic Sn complexes

Cellulose supported dendritic Sn complexes were prepared by solid phase synthetic methodology. A series of cycloketones and acyclic ketones including 2-andamantanone, cyclohexanone, 4-methylcyclohexanone, 4-tert-butylcyclohexanone, 3-methyl-2-pentanone, 4-methyl-2-pentanone and cyclopentanone were oxidized by hydrogen peroxide in a reaction catalyzed by cellulose-supported dendritic Sn complexes, affording the corresponding lactones or esters with the conversion of 70–99% and the product selectivity of 100%. The catalysts can be recycled for several times without any significant decline in catalytic activity.     

Study on a green synthetic method of TRPPMCl (M= Fe,Mn, Co)

A green synthetic method using mixted solvents of di-methyl formamide(DMF) and acids instead of single DMF to synthesize metalloporphyrins(TRPPMCl) from TRPPH₂ and MCl₂ metallization was proposed in this paper. A series of TRPPMCl (M= Fe, Mn, Co) were synthesized through this innovative synthetic method, and these complexes were characterized with various spectroscopic techniques, including IR and UV-Vis spectroscopy. The results showed that the metallization time was markedly reduced from about 10 h to 0.5 h in contrast with the conventional synthetic methods.     

相转移催化法合成乙酸苄酯的研究进展

本文简要介绍了乙酸苄酯的应用、性能特点及合成方法,着重阐述了合成乙酸苄酯的相转移催化原理及目前国内相转移催化合成乙酸苄酯的研究现状。     

Study on a green synthetic method of TRPPMCl (M = Fe, Mn, Co)

A green synthetic method using mixted solvents of di-methyl formamide (DMF) and acids instead of single DMF to synthesize metalloporphyrins (TRPPMCl) from TRPPH₂ and MCl₂ metallization was proposed in this paper. A series of TRPPMCl (M = Fe, Mn, Co) were synthesized through this innovative synthetic method, and these complexes were characterized with various spectroscopic techniques, including IR and UV-Vis spectroscopy. The results showed that the metallization time was markedly reduced from about 10 h to 0.5 h in contrast with the conventional synthetic methods.     

Purification of ice structuring protein complexes from winter wheat using Triton X-114 phase partitioning

Ice structuring proteins (ISPs) isolated from the cold-acclimated plants have a great potential in improving the quality of frozen foods. The purification of ISP complexes from winter wheat was achieved using an aqueous two-phase system of Triton X-114. The highly reactive phenols were removed, and the ISP complexes remained in the aqueous phase after phase separation. The ISP complexes treated by this procedure retained higher thermal hysteresis activity than those treated by ammonium sulfate method. The phase separation technique provides a simple and mild way for removing phenols from ISP complexes.