三(2-氨基乙基)胺-镉(Ⅱ)-2-甲基咪唑三元配合物的合成、结构与抗微生物活性

The complex [Cd(tren)(meim)](ClO₄)₂ was synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. The compound crystallizes in monoclinic system, space group P2₁/m with a=0.786 8(2) nm, b=0.834 2(2) nm, c=1.496 2(4) nm, M_r=538.64, Z=2, F(000)=542, D_c=1.822 g·cm^-3, T=298(2) K, μ=1.435 mm^-1 and λ=0.071 073 nm. The structure was refined to R=0.045 8 and wR=0.123 1 for 1 489 observed reflections with I>2σ(I). The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method. It was found to be active against the four test bacterial organisms. CCDC: 600198.     

聚酰胺-胺(PAMAM)树状大分子对甲氨蝶呤的包合及缓释研究

以甲氨蝶呤(MTX)为模型药物,研究了G5.0PAMAM树状大分子对其包合和释放,并用13^CNMR对PAMAM-MTX包合物进行了表征.UV-Vis研究结果表明,1个G5.0PAMAM树状大分子能包合27个MTX分子,体外释放研究表明,在37℃,pH=7.4的10mmol/LTris-HCl缓冲溶液中G5.0PAMAM树状大分子对MTX具有明显的缓释作用.     

新试剂2-(2-苯并噻唑偶氮)-5-氨基苯甲酸的合成及与钯(Ⅱ)的显色反应研究

合成了新试剂2 (2 苯并噻唑偶氮) 5 氨基苯甲酸(BTABA),研究了该试剂与钯(Ⅱ)的显色反应。于pH4.5的乙酸盐缓冲溶液中,形成了配位比为Pd∶BTA BA=1∶2的红褐色配合物,其最大吸收波长为603nm,表观摩尔吸光系数ε为6.56×104L·mol-1·cm-1。钯元素含量在0～25.0μg/25mL范围内服从比耳定律。方法应用于Pd C催化剂样品中钯元素含量的测定,结果令人满意。     

Cu2+对联苯甲醛修饰的树状大分子聚酰胺-胺荧光性能的影响

采用小分子联苯甲醛(BPA)分别修饰第一和第二代树状大分子聚酰胺-胺(PAMAM), 合成了2种PAMAM的修饰产物G1-BPA4和G1-BPA8. 利用IR, 1H NMR及MALDI-TOF MS等手段表征了2种产物的结构, 研究了Cu2+浓度对其荧光性能的影响. 结果表明, 在一定的浓度范围内, 作为常见荧光猝灭剂的Cu2+能使2种产物的荧光均显著增强.     

N,N-二(2-羟乙基)-2-氨基乙磺酸钠的合成研究

采用二乙醇胺与2-氯乙基磺酸钠反应合成N,N-二(2-羟乙基)-2-氨基乙磺酸钠(BES钠盐),由核磁氢谱(1H NMR)和碳谱(13C NMR)、红外光谱(FT-IR)、X射线衍射(XRD)等仪器表征了合成产物的结构和特性.根据反应体系pH值的变化及核磁谱图,确定了BES钠盐的最佳合成工艺:反应物料比为1:1:1,反...     

相转移催化与微波辐射合成三(2-氰乙基)胺

将微波辐射与相转移催化技术相结合,在加压密闭容器中,以氨水和丙烯腈合成了配位中间体三(2-氰乙基)胺,产率为61.2%,合成时间比传统方法缩短了8倍;在微波辐射下,产率为67.2%,合成时间缩短约90倍.对产物进行了元素分析,IR,¹H-NMR,ES-MS,及TG-DTA表征.     

新显色剂2-(2-咪唑偶氮)-5-二甲氨基苯甲酸与镍(Ⅱ)的显色反应研究

研究了新显色剂2-(2-咪唑偶氮)-5-二甲氨基苯甲酸(IZDBA)与Ni(Ⅱ)的显色反应。结果表明,在pH 6.0的HAc-NaAc缓冲溶液中,IZDBA可与Ni(Ⅱ)形成一种配合比为2∶1的稳定红色配合物,其最大吸收波长位于580 nm处,而试剂的最大吸收波长为390nm,对比度为190 nm。配合物的表观摩尔吸光系数为2.95×104L.mol-1.cm-1;Ni(Ⅱ)量在0~0.8 mg/L范围内遵守比耳定律。在硫脲和氟化铵存在下,方法可直接用于测定镍催化剂和铸造铝合金中的微量镍。本法与原子吸收光谱法相对照,结果基本一致。     

AlCl3催化3-(2-氨基乙基)吡咯的合成

3-(2-氨基乙基)吡咯是形成6-氮杂吲哚骨架的重要中间体,由于吡咯2位为高活性位点,难以直接通过傅克反应合成3-(2-氨基乙基)吡咯.报道了在吡咯α位引入拉电子基团,形成对角β位的定位效应,以无水AlCl3为催化剂,通过傅克反应在吡咯3位加成硝基烯烃,进而得到取代的3-(2-氨基乙基)吡咯.     

新试剂2-(2-苯并噻唑偶氮)-5-氨基苯甲酸与铂(Ⅳ)的显色反应研究

合成了新试剂2-(2-苯并噻唑偶氮)-5-氨基苯甲酸(BTABA),研究了新试剂与铂(Ⅳ)的显色反应,先后在pH 4左右的乙酸盐缓冲及H2SO4和H3PO4混合介质中,在表面活性剂CTMAB存在下,形成了配位比为Pt(Ⅳ)∶BTABA=1∶2的红褐色配合物,其最大吸收波长为612 nm,表观摩尔吸光系数为1.12×105L.mol-1.cm-1。铂含量在0~30.0μg/25 mL范围内服从比耳定律。应用于Pt-C催化剂中铂的测定,结果满意。     

显色剂2-(1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸与镍的显色反应研究

研究了显色剂2-(1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸(TZDBA)与镍的显色反应,试剂与镍在pH 5.0的HAc-NaAc缓冲溶液中形成紫红色配合物,组成比为n(Ni2 )∶n(TZDBA)=1∶2,配合物表观摩尔吸光系数ε=3.82×104 L·mol-1·cm-1.镍质量浓度在0～0.8 mg/L范围内符合比尔定律.配合物形成后在强酸溶液中能稳定存在,有良好的选择性.方法不经分离直接测定铝合金和纯镁中的微量镍,测定结果与认定值相符.     

Tris-(2-aminoethyl) amine as a novel and efficient tripod ligand for a copper(I)-catalyzed C-O coupling reaction

We have introduced a novel, efficient, commercially available and economically attractive N-donor tripod ligand, tris-(2-aminoethyl)amine for copper-catalyzed Ullmann diaryl ether synthesis. This catalyst system is highly active for both aryl iodides and aryl bromides. Variously substituted diaryl ethers have been synthesized in good to excellent yields.     

Synthesis and Crystal Structure of a [Cu(HTren)Cl_2]ClO_4·H_2O Complex (Tren = Tris(2-aminoethyl)amine)

1INTRODUCTION Investigation of the coordination chemistry of copper(II)continues to be stimulated by interest in developing modes for copper proteins and in under-standing the factors which give rise to the seemingly infinite variety of distortions from regular stereo-chemistry observed in Cu(II)complexes[1,2].For more than decades,due to the unique coordination polyhedra and their easy preparation,tripodal copper complexes have attracted much attention in addition to their special chemi…     

Encapsulating ruthenium and osmium with tris(2-aminoethyl)amine based tripodal ligands

The reaction of a series of tripodal ligands, H₃L^1,2 and L^3-6, with [M(PPh₃)₂Cl₂] (M = Ru, Os) affords a family of coordination cage compounds of the type [M^IIIL^1,2] (1-4) or [M^IIL^3-6](BPh₄)₂ (5-12). The Schiff base ligands (H₃L¹, L³, L⁵) have been synthesized by condensation of tris(2-aminoethyl)amine with salicylaldehyde, pyridine-2-aldehyde and 1-methyl-2-imidazolecarboxaldehyde. These ligands were further reduced and subsequently methylated to form the new ligands (H₃L², L⁴, L⁶). Single crystal X-ray diffraction studies of 1 and 2 show that the tripodal ligand wraps around the metal center as a hexadentate ligand to form a cage. All the synthesized compounds have been thoroughly characterized by ESI-MS, FT-IR, UV-Vis and NMR spectroscopic methods. To the best of our knowledge, this is the first ever report of osmium complexes with tris(2-aminoethyl)amine based tripodal ligands. DFT calculations were performed to obtain geometry optimized structures of all the other complexes (3-12).     

An efficient tris-(2-aminoethyl)amine-CuI-catalyzed thioetherification of thiols with aryl halides

A robust method has been developed to couple a wide variety of thiols and aryl halides. The C-S bond forming reaction makes use of catalytic copper(I) iodide and the ligand tris-(2-aminoethyl)amine. These conditions tolerate a wide degree of functionality on both aryl halide and thiol reactants and have resulted in numerous examples being synthesized. Commercial availability of the ready to use, inexpensive ligand, tris-(2-aminoethyl)amine and air-stable CuI make the method well suited to generate a diverse array of diaryl thioethers.     

Synthesis,Structure and Biological Activity of Zn(II) Complex with Tris(benzimidazol-2-yl-methyl)amine Ligand

Introduction Since the structures of superoxide dismutase (SOD) which appears to play an important role in both the animal and plant kingdoms to eliminate ·2O- and pro-tect living organisms from toxicity of ·2O- 1, exhibit that most of the coordinated atoms around metal ions are from imidazole groups of histidines which are the primary ligands in distorted coordination geometry2-4 in SOD, an important step should be designed to synthe-size the model compounds of SOD in which ligands shou…     

PAMAM分子与 Cr3+离子配位作用的研究

利用外向分散合成法合成了以乙二胺为核的聚酰胺-胺(PAMAM)树枝形分子,并用分光光度法研究了不同代数的PAMAM分子与Cr^3 的配位作用。实验结果表明PAMAM分子的代数、浓度以及水溶液的pH值对配位作用有显著的影响。随着PAMAM分子代数的增加,其与Cr^3 的最大配位数不断增加,得出的结果和理论值接近。     

微波衍生-离子对高效液相-磺化四苯基卟啉光度法同时测定痕量镍、铜、锰和锌

 用磺化四苯基卟啉 (TPPS4 )作柱前衍生试剂 ,在微波作用下进行衍生反应 ,研究了衍生和分离Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的最佳条件。在 75 0W的微波作用下衍生反应 3min ,在C18柱上采用乙腈 水 (体积比为 2 2 5∶77 5 )体系作流动相 ,四乙基溴化铵 (TEABr)作离子对试剂 ,在 415nm处检测 ,建立了微波衍生 离子对高效液相快速分离、光度检测Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的新方法。络合物和反应试剂在 15min内出峰完毕。Zn2 + ,Cu2 + ,Ni2 + 和Mn2 + 的检测限分别为 0 0 5 μg/L ,0 0 1μg/L ,0 10 μg/L和 0 40 μg/L。     

聚酰胺-胺树形大分子的合成与应用

聚酰胺_胺 (PAMAM)树形大分子是一种从中心核开始增长 ,具有确定代数和末端基的新型合成高分子。由于该化合物具有高度的几何对称性、大量的端基、分子内存在空腔等结构特点 ,在催化、医药、生命科学、工业等领域具有广泛的应用前景。本文通过介绍PAMAM树形大分子的合成、表征方法及其性能研究 ,讨论了其改性研究和应用。     

表面活性剂增溶比率荧光Zn2+检测方法研究

合成了一种新的Zn2+荧光检测试剂8-(2-(十八氨基)乙酰氨基)喹啉(AQZ-18)。通过自发荧光的非离子表面活性剂OP-10增溶AQZ-18,获得了一个与Zn2+结合后在320 nm和505 nm分别有两个荧光发射峰的溶液体系。短波长荧光峰来自OP-10,荧光峰强度不随Zn2+浓度变化;长波长荧光峰来自AQZ-18,荧光峰强度随Zn2+浓度增加而增强。利用上述两个荧光峰强度随Zn2+浓度变化时的比值变化建立了一种新的比率荧光Zn2+检测方法。研究表明,Zn2+与AQZ-18形成1∶1型基态配合物,其表观结合常数为1.1×106L/mol。常见金属离子对Zn2+荧光检测无干扰,Zn2+浓度在0～1.1×10-5mol/L范围内与荧光强度变化的比值呈良好的线性关系,相关系数(r2)为0.996 2,检出限为55 nmol/L。该方法可用于水样中Zn2+的检测。     

Structures of Mn(II) complexes of bis(2-pyridylmethyl)amine (bpa) and (2-pyridylmethyl)(6-methyl-2-pyridylmethyl)amine (Mebpa): geometric isomerism in the solid state

The crystal structures of [Mn(bpa)₂](ClO₄)₂ (1), [bpa?=?bis(2-pyridylmethyl)amine], and Mn(6-Mebpa)₂(ClO₄)₂ (2), [6-Mebpa?=?(6-methyl-2-pyridylmethyl)(2-pyridylmethyl)amine] have been determined. In 1, two facial [Mn(bpa)₂]²⁺ isomers are observed in the same unit cell, one with C _i (1a) and the other with C₂ (1b) symmetries. In 2, only the isomer with C₂ symmetry is observed. The structure of [Mn(bpa)₂]²⁺ with only C₂ symmetry has been reported previously (Inorg. Chem., 31, 4611 (1992)). The bond length order Mn–N_amine?>?Mn–N_pyridyl, observed in the C₂ and the C _i isomers in the crystals of 1, is the reverse of the order observed in the structure of [Mn(bpa)₂](ClO₄)₂ which contains only the C₂ isomer in the unit cell. The structure of 2 in which only the C₂ isomer is found, also shows the bond length order Mn–N_pyridyl?>?Mn–N_amine. In cyclic voltammetric experiments in acetonitrile solutions, 1 and 2 show irreversible anodic peaks at E _p?=?1.60 and 1.90?V respectively, (vs. Ag/AgCl), assigned to the oxidation of Mn(II) to Mn(III). The substantially higher oxidation potential of 2 is attributable to a higher rearrangement energy in complex 2 due to the steric effect of the methyl substituent.