双端8-羟基喹啉配体的合成与表征

设计了以8-羟基喹啉为原料,经过氯甲基化后分别与哌嗪、十二胺、癸二醇反应,合成了3种端基为8-羟基喹啉的双端配体,即N,N'-双(8-羟基喹啉基5-亚甲基)哌嗪、N,N-双(8-羟基喹啉基5-亚甲基)十二胺、O,O'-双(8-羟基喹啉基-5-亚甲氧基)癸烷.通过元素分析、核磁共振谱对3种化合物的组成和结构进行了表征.     

新型三脚架结构席夫碱及其过渡金属配合物的合成与性质

三{2-[(2-甲酰基苯基)氧代]乙基}胺与乙醇胺缩合得到一种新型席夫碱配体,然后与Cd、Mn、Co、Ni、Fe、Cu过渡金属配位得到其配合物,经元素分析、红外光谱、紫外光谱、核磁共振谱表征,确定了配体及配合物的组成,并对配体及配合物杀菌活性进行了研究.     

可高分子化的小分子8-羟基喹啉金属配合物的合成与表征

通过8-羟基喹啉的氯甲基化,预先合成5-氯甲基-8-羟基喹啉,在催化剂无水醋酸钠的作用下,再使之与双官能团的化合物氯乙醇反应,合成具有反应活性点的8-羟基喹啉的衍生物(C lCH2CH2OCH2-Hq),然后与含有A l3+,Zn2+,L i+的金属化合物及8-羟基喹啉经由配位反应,合成了可溶性的具有单反应活性点的小分子8-羟基喹啉金属配合物(这些配合物含有A lQ3,ZnQ2,L iQ基团),这类化合物可以接枝到高聚物上,得到高相对分子质量的含8-羟基喹啉金属配合物的发光材料1。HNMR、FTIR、元素分析确定了小分子8-羟基喹啉金属配合物的组成;紫外吸收光谱(UV)、光致发光光谱(PL)说明小分子8-羟基喹啉金属配合物的发光来自于A lQ3,ZnQ2,L iQ基团。     

配合物Zn(5-硝基-8-羟基喹啉)_2的合成、结构及荧光性质

以4-[(8-羟基-5-喹啉)偶氮]苯磺酸与氯化锌为原料,采用溶剂热法通过原位反应合成标题配合物,并通过X-射线单晶衍射、红外光谱、元素分析和粉末X-射线衍射等方法对其进行了表征。标题配合物中两个5-硝基-8-羟基喹啉与Zn离子配位形成离散结构,通过两种C—H…O氢键将标题配合物连接形成二维层状结构,相邻层之间借助喹啉环间的两种π…π堆积相互作用将二维超分子层状结构沿c轴连接形成了三维超分子网络结构。荧光光谱表明,标题配合物为配体到配体的跃迁,跃迁过程中伴随有分子内电荷转移。     

8-羟基喹啉衍生物的光谱性质模拟与预测

采用密度泛函理论(DFT)中的B3LYP/6-311G**方法对2-甲酰基-8-羟基喹啉、5-甲酰基-8-羟基喹啉及7-甲酰基-8-羟基喹啉进行了理论计算与分子模拟,结果表明理论计算与模拟的红外光谱吸收峰和核磁共振化学位移与实验值高度吻合。并对尚未有文献报道的3、4和6位甲酰基取代的8-羟基-喹啉衍生物光谱性质进行了理论预测。     

一种新型席夫碱及其铜配合物的合成与抑菌活性的研究

在非水溶荆中合成出一种未见报道的新型席夫碱试剂1-对氯苯基-3-苯基-4-呋喃甲酰基-吡唑酮-5缩糠胺(L)及其铜配合物.由元素分析、质谱和摩尔电导值推测出配合物的组成为CuL2,通过红外光谱、紫外先谱和核磁共振氢谱等对配体争配合物进行了结构表征并做了初步的抑茵活性实验.结果表明,配体以酮式和烯醇式共存,配位时完全异构化为酮式结构,通过吡唑啉酮环羰基上O原子和亚胺基上的N原子以双齿形式与中心离子成键,配合物的配位数为4;配合物对枯草杆茵、大肠杆菌、大肠杆菌(101)和金黄色葡萄球茵的抑制作用较配体更强.     

2-羟基-1-萘甲醛缩2,6-二氨基吡啶钍的席夫碱配合物的合成及其抑菌活性的研究

合成了2-羟基-1-萘甲醛缩2,6-二氨基吡啶席夫碱配体L,与硝酸钍反应,生成配合物ThL,研究了配体L和配合物ThL的抗菌活性。结果表明,配体L和配合物ThL对枯草杆菌、大肠杆菌、乳酸菌有良好的抑制作用,配合物ThL的抑菌活性好于配体L,最佳抑菌活性浓度是5 mmol/L。     

2-(2-羟基苯乙烯基)-8-羟基喹啉及其金属配合物的合成与光致发光特性

报道了一种2-(2-羟基苯乙烯基)-8-羟基喹啉配体(Ⅰ)及其相应金属配合物的合成,产物经IR,UV,1HNMR,元素分析等进行表征;测定了配合物Al(Ⅰ)2,Zn(Ⅰ)2的荧光性质,Al(Ⅰ)2,Zn(Ⅰ)2在光致发光谱中λmax分别为573.0,547.0 nm。     

2-（4-咪唑基苯乙烯基）-8-羟基喹啉锌的合成与光致发光特性

合成了一种新型的2-（4-咪唑基苯乙烯基）-8-羟基喹啉配体以及其金属锌配合物,用红外光谱（IR）、紫外光谱（UV）、元素分析（EA）、核磁共振氢谱（1H NMR）等确认了化合物的结构,通过荧光光谱测定了配合物的荧光性质,证实其具有良好的光致发光性能,最大发射波长为576 nm;热重分析实验也表明了金属锌配合物有很好的热稳定性。     

5-甲基-4-噁异唑-3-甲基-2-噻吩甲酰腙及其 Co（Ⅱ）配合物的合成与表征

以5-甲基-4-噁异唑甲酰肼为原料,与3-甲基-2-噻吩甲醛反应合成5-甲基-4-噁异唑-3-甲基-2-噻吩甲酰腙,再将其作为配体与钴离子合成相应的钴配合物,对其进行红外、核磁共振氢谱、紫外-可见等表征确认结构,并对配体及其配合物的荧光性能进行测定。荧光测定表明,配体及其配合物都较强的荧光性能,因此可作为潜在的光活性材料。     

Synthesis,Characterization and Material Application of Novel Polyimide

Novel polyimide-II containing 8-hydroxyquinoline as pendent groups was prepared by reacting N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide--diamine polyimide-I (BPBMDDM) with 5-chloromethyl-8-hydroxyquinoline hydrochloride (CMHQ) in the presence of base catalyst. N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide--diamine polyimide-I (BPBMDDM) was prepared by Michael addition reaction of N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide (BPBM) with 4,4′-diaminodiphenyl methane (DDM). The resulting polyimide-II (BPBMDDMCMHQ) was characterized by spectral techniques. Polymeric metal chelates of polyimide-II were prepared using the transition metal ions Zn(II), Cu(II), Ni(II), Co(II), and Mn(II), and were characterized. Ion-exchange properties of polyimide-II (BPBMDDMCMHQ) for Fe(III), Zn(II), Ni(II) and Cu(II) metal ions were also studied by batch-equilibration method. The polyimide-II (BPBMDDMCMHQ) has good metal uptake capacity at varying pH range and can be recycled. It has thermal stability up to 240°C.     

Oligoimide Containing 8-Hydroxyquinoline as a Pendent Group

New ethylenebismaleimide-diamine oligoimide-II (EBMDDMCMHQ) containing 8-hydroxyquinoline as a pendent group(s) was prepared using ethylenebismaleimide-diamine oligoimide-I (EBMDDM) and 5-chloromethyl-8-hydroxyquinoline hydrochloride (CMHQ) in the presence of base catalyst. Ethylenebismaleimide-diamine oligoimide-I (EBMDDM) was prepared by the Michael addition reaction of ethylenebismaleimide (EBM) and 4,4′-diaminodiphenyl methane (DDM). The resulting oligoimide-II (EBMDDMCMHQ) was characterized by spectral techniques. Polymeric metal chelates of oligoimide-II were prepared using transition metal ions and were duly characterized. Ion-exchange properties of oligoimide-II for Fe(III), Zn(II), Ni(II), and Cu(II) metal ions were also studied by batch-equilibration method. It has good metal ion uptake capacity at varying pH ranges.     

Synthesis, spectral characterisation and antimicrobial activity of new disazo dyes derived from heterocyclic coupling components

Two series of new disazo dyes were prepared by diazotising 4,4'-diaminodiphenylsulphonamide and 4,4'-diaminodiphenylurea and coupling with 3-methyl-1-phenyl-pyrazoline-5-one, 2-methylindole, 8-hydroxyquinoline, 2-phenylindole, 1-methyl-2-phenylindole, 3-amino-1-phenyl-pyrazoline-5-one. These dyes were characterised by ultraviolet–visible, Fourier transform infrared, nuclear magnetic resonance spectroscopic techniques and elemental analysis. The spectral characterisation of the dyes was evaluated with respect to visible absorption properties in various solvents. The effects of acid and base on the visible absorption maxima of the dyes were also reported. In addition, the antimicrobial effect of the dyes was evaluated.     

Synthesis and properties of new poly(amide‐imide)s based on 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane and aromatic diamines

Six new poly(amide‐imide)s 8a–f containing trimethylene moiety in the main chain were synthesized by the polycondensation reactions of 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane 6 with six different aromatic diamines 7a–f in a medium constituting N‐methyl‐2‐pyrrolidone, triphenylphosphite, CaCl₂, and pyridine as condensing agents. The polycondensation reaction produced a series of novel poly(amide‐imide)s 8a–f in high yields with inherent viscosities between 0.35 and 0.63 dL/g. The resulting poly(amide‐imide)s were characterized by elemental analysis, viscosity measurements, thermal gravimetric analysis (TGA and DTG), solubility tests, and FTIR spectroscopy. 1,3‐Bis[4,4'‐(trimellitimido) phenoxy] propane 6 as a new monomer containing trimethylene moiety was synthesized using a three‐step reaction. At first 1,3‐bis[4,4'‐nitrophenoxy] propane 3 was prepared by the reaction of 4‐nitrophenol 1 with 1,3‐dibromo propane 2 in DMF solution . Then, dinitro 3 was reduced to 1,3‐bis[4,4'‐aminophenoxy] propane 4 by using a solution of sodium sulfite in ethanol. Finally, 1,3‐bis[4,4'‐(trimellitimido) phenoxy] propane 6 was prepared by the reaction of one equivalent diamine 4 with two equivalents of trimellitic anhydride 5 in a mixture of acetic acid‐pyridine (3 : 2). © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

New photosensitive poly(amid‐imide)s containing chalcone moiety and hydantoin derivatives in the main chain: Synthesis and characterization

Six new poly(amid‐imide)s containing chalchone and hydantoin moieties in the main chain were synthesized through the polycondensation reaction of 1,3‐bis[4,4′‐bis(trimellityimido)phenyl]‐2‐propenone 6 with six hydantoin derivatives 7a‐f in a medium consisting of triphenyl phosphite, calcium chloride, pyridine, and N‐methyl‐2‐pyrrolidone. The polycondensation reaction produced a series of novel poly(amid‐imide)s 8a‐f in high yields with inherent viscosities between 0.26 and 0.42 dL/g. The resulting polymers were characterized by elemental analysis, viscosity measurements, solubility test, thermo gravimetric analysis (TGA and DTG), FTIR, and UV‐Vis spectroscopy. 1,3‐bis[4,4′‐bis(trimellityimido)phenyl]‐2‐propenone 6 was prepared from a three‐step reaction by using 4‐nitro benzaldehyde 1 and 4‐nitro acetophenone 2 as precursors. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and characterization of curable methacrylate‐based monomers

The synthesis of new methacrylate‐based, curable macromonomers, 4,4′‐bis[2‐hydroxy‐3‐aminopropylmethacrylate] diphenyl ether (BHAPE) and 4,4′‐bis[2‐hydroxy‐3‐aminopropylmethacrylate] diphenyl methane (BHAPM), is reported. BHAPE and BHAPM were prepared by the reaction of glycidyl methacrylate (GMA) with 4,4′‐diaminodiphenyl ether and 4,4′‐diaminodiphenyl methane, respectively. The progress of the reaction was monitored by thin‐layer chromatography (TLC), and the structure of the monomers was characterized by Fourier transform infrared (FTIR) and ¹H‐NMR spectroscopy. Thermal curing of the monomers was conducted in a differential scanning calorimeter (DSC) with peroxide as the initiator. Thermal curing of the monomers showed the highest rate at 100°C with the activation energy value in the range 80–90 kJ distilled/mol. The water absorption properties of the cured samples in water, acidic, and basic solutions were studied. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Amino-p-benzoquinone Adducts and Polymers as Adhesion Promoters for Steel

Phenolic and quinonoid compounds are widely studied in biological sciences because of their ability to chelate heavy metals like iron and copper and recently have found new applications in synthetic macromolecules. Amino-p-benzoquinone polymers, poly[(2,5-hexamethylenediamino)-1,4-benzoquinone] and poly{[2,5-(2,2′-bistrifluoromethyl)-4,4′-biphenylenediamino]1,4-benzoquinone} were synthesized and evaluated as adhesion promoters for steel/epoxy joints. An improvement in the torsional shear strength of these joints was observed when these polymers were used as adhesion promoters. The durability of the adhesive bond was also improved after boiling water treatment, relative to untreated and silane-treated joints. The improvement in adhesion could be attributed to the formation of a chelate between the polyaminoquinone (PAQ) and the iron surface and a chemical reaction between the PAQ and the epoxy resin. A low molecular weight model compound, bis[2,5-(4-methylanilido)]-1,4-benzoquinone, was also used to study coupling between the epoxy adhesive and the steel surface. Electron spin resonance (ESR), atomic absorption spectroscopy and infrared spectroscopy were used to document the epoxy-coupling agent reaction and the chelate formation.     

7-(4-安替吡啉偶氮)-8-羟基喹啉的合成及与铟的显色反应

合成了7-(4-安替吡啉偶氮)-8-羟基喹啉,考察了滴加顺序、反应温度、偶合反应时间、溶剂对反应的影响。产物的结构经红外光谱及核磁共振谱进行表征。研究在pH4.5的NaAc-HAc缓冲介质中显色剂与In( )的显色反应特性。结果表明:试剂与In( )形成3∶1的黄色配合物,配合物的最大吸收波长位于482nm,表观摩尔吸光系数ε=1.9×104L/(mol·cm),铟的浓度在0～20μg/25mL范围内符合比耳定律。     

Synthesis and characterization of novel ion-exchange resin based on polyimide containing 8-hydroxyquinoline as a pendent groups

Novel ion-exchange resin (PBMDDMCMHQ polyimide) having 8-hydroxyuinoline as a pendent groups was prepared using phenylenebismaleimide-diamine polyimide (PBMDDM) and 5-chloromethyl-8-hydroxyquinoline hydrochloride (CMHQ). Phenylenebismaleimide-diamine polyimide (PBMDDM) was prepared by Michael addition reaction of 1,3-phenylenebismaleimide (PBM) and 4,4’-diaminodiphenyl methane (DDM). The resulting ion-exchange resin was characterized by spectral techniques. Polymeric metal chelates of ion-exchange resin were also prepared using transition metal ions Zn(II), Cu(II), Ni(II), Co(II) and Mn(II), and were duly characterized. Ion-exchange properties of ion-exchange resin (PBMDDMCMHQ) for Fe(III), Zn(II), Ni(II) and Cu(II) metal ions were also studied by batch-equilibration method. The produced ion-exchange resin (PBMDDMCMHQ) has thermal stability up to 220°C and can be used over a wide pH range. It has good metal up take capacity at varying pH range and can be recycled.