共查询到19条相似文献,搜索用时 93 毫秒
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一种1,10菲啰啉-5,6-二酮及其单肟的高效合成方法 总被引:2,自引:0,他引:2
1,10菲啰啉5,6二酮(2)与1,10菲啰啉5,6二酮单肟(3)作为稠杂环共轭配体,既具有良好的配位特性,又是重要的有机合成反应中间体。由化合物2和它的衍生物与金属离子形成的配合物可以用于抗肿瘤药物、DNA探针、非线性光学材料、超分子组装分子骨架、自旋交叉配合物等许多领域。化合物3则用于有机光致变色化合物螺噁嗪的合成。化合物2无法直接用氧化剂氧化1,10菲啰啉(1)得到。它最初是从化合物1用混酸硝化制备5硝基1,10菲啰啉的废水中分离得到的,产率1%。Amouyal等[1]改进此方法,将产率提高到20%。随着应用研究的需求,对它的合成研究一直没有间… 相似文献
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以2,9-二氯-1,10-邻菲啰啉-5,6-二酮为原料,与2-硝基丙烷反应得双酮被保护的2,9-二氯-5,6-O-异丙叉基-1,10-邻菲啰啉(2);2与频哪醇硼酸酯在PdCl2(dppf)催化下经Miyaure反应合成了新化合物———9,9'-二氯-5,6;5',6'-二(O-异丙叉基)-2,2'-联邻菲啰啉,其结构经1H NMR,IR和MALDI-TOF-Mass表征。 相似文献
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报道了二氰基二硫纶·菲咯啉 5,6 二酮混配钴(Ⅱ)配合物CoLL′(L=mnt2-.mnt2-为1,2 二氰基乙烯 1,2 二硫醇离子.L′=phen 5,6 dione,1,10 菲咯啉 5,6 二酮)的合成和标题配合物的电子吸收光谱、电子发射光谱.研究了CoLL′对CdS的光敏化作用与其电子光谱间的关系. 相似文献
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由1,10-邻菲咯啉合成1,10-邻菲咯啉-5,6-二酮反应的副产物的形成与控制研究表明,1,10-邻菲咯啉在5,6位二酮化反应中的副反应产物及主产物分离时产生的副产物均为4,5-二氮杂芴-9-酮,二酮化反应条件(包括作为氧化剂的强混合酸H2SO4/HNO3的加入量、时间和温度)和主产物分离时体系的酸度对副产物的形成有重要影响,优化了二酮化反应条件和产物分离时的体系pH控制范围。在此优化条件下,可有效控制副产物的形成,使主产物1,10-邻菲咯啉-5,6-二酮的收率达到92%以上。 相似文献
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以1,10-邻菲啰啉-5,6-二酮(phendio)修饰碳糊电极为工作电极,在0.05mol/L HAc-NaAc(pH4.74)电解液中,于-1.30V(vs.SCE)处Cd2 以Cd-1,10-邻菲啰啉-5,6-二酮络合物的形式吸附到电极上,再经过阳极溶出,从而建立了一种测定水样中痕量镉的新方法。本法于-0.69V处产生一个灵敏的溶出峰,其二阶导数峰电流与Cd2 的浓度在2.4×10-7~6.0×10-9mol/L范围内呈良好的线性关系;检出限为3.0×10-10mol/L(S/N=3)。应用本方法测定水样中的Cd2 ,结果令人满意。 相似文献
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基于1,10-菲咯啉-5,6-二酮2,9位双噻吩的扩展策略,设计合成了2个化合物1和2。有趣的是,在大位阻双齿螯合配体2的配位化学研究中发现,只有铜( Ⅱ)离子生成了稳定的配合物3·H2O。此外,对2,2·CHCl3和3·H2O的X-射线单晶结构研究表明,为了克服空间位阻以满足中心铜( Ⅱ)离子的配位构型要求,1,10-菲咯啉-5,6-二酮及其2,9位取代的2个噻吩环之间的二面角分别从自由配体中的1.9(2)°、5.2(6)°和25.3(3)°、34.9(3)°增加到了铜( Ⅱ)配合物中的5.6(2)°、6.5(6)°和27.2(3)°、38.2(3)°。 相似文献
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过渡金属离子与3-氟邻苯二甲酸(H2Fpht)、1,10-邻菲啰啉(phen)通过水热反应得到了5个配合物:[M(Fpht)(phen)(H2O)3]·H2O(M=Ni 1,Co 2),[Cu(Fpht)(phen)(H2O)]·H2O(3),[M(Fpht)(phen)(H2O)]·H2O(M=Zn 4,Cd 5)。通过X-射线单晶衍射分析、元素分析、红外分析、荧光分析以及差热-热重分析对配合物进行了表征。配合物1和2为单核分子,中心离子Ni(Ⅱ)和Co(Ⅱ)与3-氟邻苯二甲酸根的1个氧原子,1,10-邻菲啰啉的2个氮原子以及3个配位水分子的3个氧原子配位,形成六配位的扭曲八面体构型。配合物3为Z字形一维链状结构。中心Cu(Ⅱ)离子与2个3-氟邻苯二甲酸根的2个氧原子,1个1,10-邻菲啰啉的2个氮原子以及水分子的1个氧原子配位,形成四方锥构型。配合物4和5具有相似的一维螺旋结构,中心Zn(Ⅱ)和Cd(Ⅱ)离子与2个3-氟邻苯二甲酸根的3个氧原子、1,10-邻菲啰啉的2个氮原子以及水分子中的1个氧原子配位,形成扭曲的八面体构型。 相似文献
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The complexation of Fe(II) and Cu(II) ions by phenanthroline and terpyridine-based Langmuir films was studied by the effect the added ions in the subphase on the isotherms. We found that Cu(II) had a pronounced effect on the isotherm consisting of phenanthroline moieties forming a square-planar 1:2 (Cu(II)/phenanthroline) complex. However, Fe(II) affected the isotherm made of 1:1 phenanthroline/terpyridine amphiphiles as a result of forming a pentacoordinate complex. 相似文献
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Bales BC Pitié M Meunier B Greenberg MM 《Journal of the American Chemical Society》2002,124(31):9062-9063
Copper-phenanthroline complexes and their conjugates are useful reagents for studying nucleic acid interactions. Although DNA cleavage by such complexes was discovered more than 20 years ago, significant questions remain unanswered regarding the chemical mechanism(s) by which DNA is damaged. Kinetic evidence is provided, which demonstrates that the major pathway for DNA damage by a minor groove binding molecule conjugated to copper phenanthroline (6) involves C1'-oxidation. Additional experiments using 6 and a DNA substrate containing 2-deoxyribonolactone (1) show that direct strand breaks are produced via beta-elimination from 1. These studies support the original mechanism for DNA damage by copper phenanthroline put forth by Sigman and a more recent proposal concerning the mechanism for direct strand break formation. 相似文献
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The title complex has been obtained by the reaction of copper nitrate trihydrate with 4-abaH (4-abaH = 4-aminobenzonic acid) and phenanthroline in ethanol solution,and its structure was determined by X-ray crystallography with the following data: monoclinic,space group C2/c, Mr = 1266.13, Cu2C52H54N10O20, a = 25.884(5), b = 10.205(2), c = 20.849(4)(A), β= 106.34(3)°, Z = 4, V= 5284.7(18) (A)3, F(000) = 2616, Dc = 1.591 g/cm3, μ = 0.896 mm-1,the final R = 0.0441 and wR = 0.1148 for 4200 observed reflections (I > 2σ(I)). In the molecule of the title complex, the asymmetric unit contains one half molecule. The Cu(Ⅱ) atom is five-coordinated by a terminal water molecule, a bidentate phenanthroline and two monodentate 4-aminobenzoate ligands forming a square pyramidal coordination environment. The two bridging 4-aminobenzoate ligands result in a dinuclear copper(Ⅱ) cluster with a short Cu-Cu distance (3.048 (A)) and a π-πstacking between the adjacent phenanthroline rings (2.96 (A)). 相似文献
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The reaction of solution 2,6‐pyridinedicarboxylic acid and 1,10‐phenanthroline ( 1 ) with CrCl3·6H2O led to the complex [Cr(phen)(pydc)(H2O)][Cr(pydc)2]·4H2O ( 2 ) (phen is 1,10‐phenanthroline and pydcH2 is 2,6‐pyridinedicarboxylic acid). 2 was characterized by elemental analysis, IR spectroscopy and single‐crystal structure determination. Crystal data for 2 at ?80 °C: triclinic, space group , a = 818.5(1), b = 1492.2(1), c = 1533.6(2) pm, α = 76.45(1)°, β = 84.22(1)°, γ = 77.99(1)°, Z = 2, R1 = 0.0416. 相似文献
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以2,4-二氯苯氧乙酸(2,4-DAA)和邻菲啰啉(Phen)为原料, 采用水热法合成了一个新的三核锌配合物Zn3(phen)2(2,4-DAA)6. 该配合物属三斜晶系, P1空间群, 晶胞参数a=1.1030(2) nm, b=1.2930(3) nm, c=1.5081(3) nm, α=100.436(3)°, β=110.227(3)°, γ=103.802(3)°, V=1.8760(7) nm3, Dc=1.661 g/cm3, Z=1, F(000)=944. 最终GooF=1.033 , 偏离因子R1=0.0326, wR2=0.0736. 在配合物分子中, 3个锌(Ⅱ)离子在同一直线上, 且以中间锌(Ⅱ)为对称中心, Zn1…Zn2的距离为0.3378 nm; 3个锌(Ⅱ) 离子存在两种配位方式: 其中对称的锌离子分别与3个2,4-二氯苯氧乙酸中的3个羧基氧原子及一个邻菲啰啉的2个N原子配位, 形成了五配位的变形四方锥结构, 而中间的锌离子与6个2,4-二氯苯氧乙酸中的6个羧基氧原子配位, 形成了六配位变形八面体结构. 研究了配合物的光谱和电化学性质. 相似文献
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Hydrothermal reactions of copper salts with fumaric acid, 1, 10‐phenanthroline or 2, 2‐bipyridine in basic aqueous solution gave rise to two mixed‐valence copper complexes [Cu4(ophen)4(fum)] ( 1 ) and [Cu4(obipy)4(fum)]·6H2O ( 2 ) (fum = fumarate dianion, Hophen = 2‐hydroxy‐1, 10‐phenanthroline and Hobpy = 6‐hydroxy‐2, 2′‐bipyridine), which were characterized by single crystal X‐ray analysis. [Cu4(ophen)4(fum)] (1) crystallizes in the monoclinic space group P21/n, with a = 10.4749(8), b = 13.4210(9), c = 15.1090(10)Å, β = 103.811(3)° Z = 2; [Cu4(obipy)4(fum)]·6H2O ( 2 ) has the triclinic space group P1¯, with a = 10.1302(11), b = 10.4406(12), c = 11.4450(13)Å, α = 84.384(2)°, β = 79.064(2)°, g = 67.734(2)° and Z = 1. The fumaric acid ligand acts as a multi‐dentate bridging ligand in both compounds, 1 and 2 , to link copper atoms into dumbbell structure. During the reactions, 1, 10‐phenanthroline and 2, 2′‐bipyridine ligands are all hydroxylated into ophen and obipy, which provide useful structural evidence for the study on the Gillard mechanism. 相似文献