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新型杂环三氮烯荧光试剂1,8-双(2-苯并噻唑重氮氨基)萘的合成及其分析应用 总被引:1,自引:1,他引:0
将1,8-萘二胺和苯并噻唑类试剂结合, 并引入杂环三氮烯结构, 合成了新荧光试剂1,8-双(2-苯并噻唑重氮氨基)萘(BBTANP), 其结构经红外光谱、核磁共振谱和元素分析证实. 研究结果表明, 在碱性介质中, 该试剂与Cu(Ⅱ)形成1∶1的络合物, 并在λex/λem=362 nm/459 nm处产生荧光增强作用. 据此建立了BBTANP测定Cu(Ⅱ)的新型荧光分析法, 该方法的线性范围为8.0×10-7—1.0×10-5 mol /L, 检测限为1.3×10-7 mol/L. 将其应用于水样中Cu(Ⅱ)的测定, 结果令人满意. 相似文献
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以9,10-二溴蒽,二苯胺等为原料经Buchwald-Hartwig芳胺化、溴化、Suzuki偶联和水解等反应合成一个新的芳香四元羧酸N,N,N',N'-四[4-(4'-羧基)联苯基)]-9,10-蒽二胺。其结构经~1H NMR,~(13)C NMR和高分辨质谱表征。初步荧光研究表明,该化合物钠盐水溶液具有发绿光的性质,最大发射波长为497 nm,同时也有较好的荧光量子效率。循环伏安法测试得到其钠盐的HOMO和LUMO分别为-5. 2 eV和-4. 4 eV。 相似文献
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5,5-二甲基-2-氧代-2-(N,N'-对苯二胺基-二苄基)- 二-1,3,2-氧磷杂环己烷的合成及表征 总被引:1,自引:0,他引:1
以新戊二醇、三氯化磷和乙醇为原料制得中间体5,5-二甲基-1,3,2-二氧磷杂环己烷-2-氧(DPDO),用DPDO)与由芳醛和对苯二胺缩合制得的席夫碱SBⅠ~SBⅢ加成,合成了膨胀型阻燃剂5,5-二甲基-2-氧代-2-(N,N′-对苯二胺基-二苄基)-二-1,3,2-氧磷杂环己烷(DPPO Ⅰ~DPPOⅢ),通过元素分析,IR,NMR和MS对其结构进行表征,并对其在醇酸清漆中的应用进行了讨论. 相似文献
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合成了一种新型的有机电致发光材料:N,N'-二苯基-N,N'-二(1-萘基)-1,5-萘二胺(NPN),测定了其吸收光谱和荧光发射光谱.该材料具有很好的热稳定性,DSC测定其玻璃化温度(Tg)高达127℃,循环伏安法(CV)测定其电离势(Ip)为5.30eV,可望用作有机电致发光空穴传输或蓝色发光材料. 相似文献
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Gan X Chi SM Mu WH Yao JC Quan L Li C Bian ZY Chen Y Fu WF 《Dalton transactions (Cambridge, England : 2003)》2011,40(28):7365-7374
Two novel facial-capping tris-naphthyridyl compounds, 2-chloro-5-methyl-7-((2,4-dimethyl-1,8-naphthyridin-7(1H)-ylidene)(2,4-dimethyl-1,8-naphthyridin-7-yl))methyl-1,8-naphthyridine (L(1)) and 2-chloro-7-((2-methyl-1,8-naphthyridin-7(1H)-ylidene)(2-methyl-1,8-naphthyridin-7-yl))methyl-1,8-naphthyridine (L(2)), as well as their Cu(i) and Pb(ii) complexes, [CuL(a)(PPh(3))]BF(4) (1) (PPh(3) = triphenylphosphine, L(a) = bis(2,4-dimethyl-1,8-naphthyridin-7-yl)(2-chloro-5-methyl-1,8-naphthyridin-7-yl)methane), [CuL(b)(PPh(3))]BF(4) (2) (L(b) = bis(2-methyl-1,8-naphthyridin-7-yl)(2-chloro-1,8-naphthyridin-7-yl)methane), [Pb(OL(a))(NO(3))(2)] (3) (OL(a) = bis(2,4-dimethyl-1,8-naphthyridin-7-yl)(2-chloro-5-methyl-1,8-naphthyridin-7-yl)methanol) and [Pb(L(b))(2)][Pb(CH(3)OH)(NO(3))(4)] (4), have been synthesized and characterized by X-ray diffraction analysis, MS, NMR and elemental analysis. The structural investigations revealed that the transfer of the H-atom at the central carbon to an adjacent naphthyridine-N atom affords L(1) and L(2) possessing large conjugated architectures, and the central carbon atoms adopt the sp(2) hybridized bonding mode. The reversible hydrogen transfer and a geometric configuration conversion from sp(2) to sp(3) of the central carbon atom were observed when Pb(II) and Cu(I) were coordinated to L(1) or L(2). The molecular energy changes accompanying the hydrogen migration and titration of H(+) to different receptor-N at L(1) were calculated by density functional theory (DFT) at the SCRF-B3LYP/6-311++G(d,p) level in a CH(2)Cl(2) solution, and the observed lowest-energy absorption and emission for L(1) and L(2) can be tentatively assigned to an intramolecular charge transfer (ICT) transition in nature. 相似文献
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以可再生资源2,5-呋喃二甲酸(FDCA)和1,8-辛二醇(1,8-ODO)为原料,钛酸四丁酯为催化剂,采用直接酯化法制得聚2,5-呋喃二甲酸1,8-辛二酯(1,8-POF)。 考察了原料配比、催化剂用量、酯化温度、缩聚温度及缩聚时间对聚合反应的影响,结果表明,当n(FDCA)∶n(1,8-ODO)=1∶1.2,钛酸四丁酯摩尔分数为0.3%,酯化温度为240 ℃,缩聚温度为260 ℃,缩聚时间为300 min时,缩聚产物的比浓粘度最高(2.1 dL/g),端羧基含量最低(5.8 mol/t)。 与乙二醇相比,采用1,8-辛二醇为单体降低了酸醇的摩尔比,减少了醇的消耗,同时得到了较高分子量的聚合物。 气质联用仪对酯化馏出液和缩聚产物真空抽出物进行了分析,结果表明,酯化馏出液的主要成分是水,并含有少量的1,8-ODO;缩聚产物真空抽出物的组成为环己酮(56%)、顺式-3-辛烯醇(18%)、4-甲基-3-戊烯-2-酮(17%)和4-羟基-4-甲基-2-戊酮(9%)。 相似文献
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The reduction of 1,8-dimethoxyanthracenedione with zinc dust and aqueous ammonia gives a mixture of 1,8-dimethoxyanthracene and 4,5-dimethoxy-9(10H)-anthracenone, rather than the isomeric 1,8-dimethoxy-9(10H)-anthracenone (dimethylanthralin). This isomer was obtained exclusively using SnCl(2) in HCl and acetic acid as reducing agent at room temperature. The structure was confirmed to exist as the tautomeric 1,8-dimethoxy-9-hydroxyanthracene. Furthermore, the reduction of 1,8-diacetoxyanthracenedione with SnCl(2) in HCl and acetic acid leads to 1,8-dihydroxy-9(10H)-anthracenone (anthralin) rather than 4,5-dihydroxy-9(10H)-anthracenone (isoanthralin), which was prepared by ether cleavage of 4,5-dimethoxy-9(10H)-anthracenone. In light of these findings some biological studies on antipsoriatic anthracenones have to be reconsidered. 相似文献
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包结物晶析法选择分离辛夷挥发油中1,8-桉叶素 总被引:6,自引:1,他引:5
主客体化学的分子识别在同分异构体选择分离、外消旋异构体光学拆分中已有广泛研究[1~3].我们利用中草药挥发油中化学组分的分子形状、几何拓扑性质、官能团数量和键力性质的不同,选定主体分子对挥发油中某一组分进行分子识别,并以结晶的形式从挥发油体系中离析出来,达到选择分离单一挥发油化学组分的目的[4~7].本文利用主体分子1,1,6,6-四苯基-2,4-己二炔-1,6-二醇(A)作为主体分子[8],以辛夷挥发油为研究对象,其主要成分1,8-桉叶素(B)为分子识别的客体分子,与化合物A形成稳定的包结物晶体(A+B),并从辛夷挥发油中析出,得到纯度为100%的… 相似文献
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Daniel L. Reger Russell P. Watson Mark D. Smith 《Journal of organometallic chemistry》2007,692(14):3094-3099
The new anthracene-based, bitopic bis(pyrazolyl)methane ligand 1,8-bis(4-[bis(1-pyrazolyl)methyl]phenyl)anthracene (1,8-[4-CH(pz)2C6H4]2C14H8) has been prepared by the cobalt-catalyzed reaction between thionyldipyrazole and 1,8-bis(4-formylphenyl)anthracene. The reaction between 1,8-[4-CH(pz)2C6H4]2C14H8 and Re(CO)5Br yielded the dirhenium complex {μ-1,8-[4-CH(pz)2C6H4]2C14H8}[Re(CO)3Br]2. The solid state structure of this complex displays extensive noncovalent interactions, particularly CH-π and π-π interactions. 相似文献
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The title complex, {[Cd2(1,8-nap)2(H2O)2](bpp)2}n(1), a cadmium complex based on mixed naphthalene-1,8-dicarboxylate (1,8-nap) and flexible 1,3-bi(4-pyridyl)propane (bpp) ligands, has been hydrothermally synthes-ized. It consists of a one-dimensional chain along c axis, which is derived from dimeric unit [Cd2(1,8-nap)2(H2O)2] linked by a pair of bpp ligands. In every [Cd2(1,8-nap)2(H2O)2] dimeric unit, two 1,8-nap act as bridging ligands to connect two Cd(Ⅱ) atoms, forming a sixteen-membered ring. Each Cd(Ⅱ) atom is in a distorted octahedral environment, coordinated by one aqua, two 1,8-nap and two bridging bpp ligands. In addition, two bridging bpp ligands connected two neighboring Cd(Ⅱ) atoms form a twenty-four-membered ring. The TGA and Luminescence property in solid state of complex 1 have been further studied and discussed in this paper. CCDC: 669293. 相似文献
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Axially chiral 1,8-bis(2,2'-diphenyl-4,4'-diquinolyl)naphthalene, 8, and 1,8-bis(2,2'-diisopropyl-4,4'diquinolyl)naphthalene N,N'-dioxide, 9, have been prepared to study the stereodynamics of these and other 1,8-diheteroarylnaphthalenes based on reversible first-order isomerization kinetics and crystallographic data. The ratio of the two enantiomeric anti-conformers to the meso syn-isomer of 8 and 9 was determined as 1.2:1 and 9.6:1. Investigation of the conformational stability of the atropisomers at enhanced temperatures using HPLC and NMR spectroscopy revealed a Gibbs activation energy of 122.4 (121.8) kJ/mol and 115.2 (109.0) kJ/mol for the anti/syn- (syn/anti)-isomerization of 8 and 9, respectively. Comparison of the conformational stability of a series of 1,8-dipyridylnaphthalenes and 1,8-diquinolylnaphthalenes shows that the latter exhibit a significantly higher rotational energy barrier. While the syn- and anti-isomers of 1,8-dipyridylnaphthalenes interconvert rapidly at room temperature the stereoisomers of 1,8-diquinolylnaphthalenes can be isolated by chromatography or crystallization and stored at 25 degrees C for several months without any sign of racemization. The conformational stability of 1,8-diquinolylnaphthalenes is a consequence of significantly increased steric hindrance to isomerization in a highly congested T-shaped transition state. Conversion of 1,8-diheteroarylnaphthalenes to their corresponding N,N'-dioxides was found to result in an increased anti/syn-ratio and decreased rotational energy barrier, which was attributed to synergistic repulsive dipole/dipole interactions destabilizing the diastereomeric ground states and facilitated out-of-plane bending reducing the steric hindrance in the T-shaped transition state. 相似文献
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Yamashita M Kamura K Yamamoto Y Akiba KY 《Chemistry (Weinheim an der Bergstrasse, Germany)》2002,8(13):2976-2979
A novel potential tridentate ligand, 1,8-bis(dimethylamino)-9-bromoanthracene, was synthesized. The key steps are as follows: 1) dimethylamination of 1,8-dibromo-9-methoxyanthracene by a modified Buchwald's method to afford 1,8-bis(dimethylamino)-9-methoxyanthracene, and 2) reduction of the methoxy group by LDBB (lithium di-tert-butylbiphenylide) followed by treatment with BrCF2CF2Br. The corresponding 1,8-bis(dimethylamino)-9-lithioanthracene, which should be a useful versatile tridentate ligand, could be generated by treatment of the bromide with one equivalent of nBuLi. The lithioanthracene reacted with B-chloroborane derivatives to give three 9-boryl derivatives. Although we recently reported that the crystal structure of 1,8-dimethoxy-9-B-catecholateborylanthracene was a symmetrical compound with the almost identical two O-B distances (2.379(2) and 2.441(2) A), the newly prepared 1,8-bis(dimethylamino)-9-borylanthracene derivatives clearly have unsymmetrical structures with coordination of only one NMe2 group toward the central boron atom. However, the energy difference between the unsymmetrical and symmeterical structures was found to be very small based on 1H NMR measurements, in which symmetrical anthracene patterns in the aromatic region (two kinds of doublets and a triplet) and a sharp singlet signal of the two NMe2 groups were observed even at -80 degrees C. 1,8-Bis(dimethylamino)-9-bromoanthracene itself can be a versatile ligand for transition metal compounds. In fact, direct palladation of the bromide took place by the reaction with [Pd2(dba)3].CHCl3 in THF to give the 9-palladated product. X-ray crystallographic analysis of the Pd compound showed that the square planar palladium atom was coordinated in a symmetrical fashion by both NMe2 groups (Pd-N bonds are 2.138(5) and 2.146(5) A). 相似文献
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The present paper covers the syntheses of 1,8-adipoylamido-bis(1,10-phenanthroline-5-yl)(bphaa) and its binuclear complex {[(bpy)2Ru]2(bphaa)}(PF6)4, where bpy is 2,2′-bipyridine. The two novel compounds were confirmed by means of elemental analysis, IR, LD-MS and 1H NMR, and 1H NMR spectra were completely assigned in virtue of 1H-1H COSY. The electrochemical behavior of the binuclear Ru(Ⅱ) complex was obtained using cyclic and square-wave voltammetry. Its photophysical property was investigated by electronic absorption, fluorescence excitation and emission spectra. 相似文献
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《Analytical letters》2012,45(3):605-612
Abstract Chromium (VI) can oxidize and decolor three colour reagents, i.e. 1,8-dihydroxy-2-(4′-chloro-2′-phosphonophenylazo)-7-(6″.8″-disulfonaphthylazo)-3,6-disulfonaphthalene (RI): 1,8-dihydroxy-2-(4′-chloro-2′-phosphonophenylazo)-7-(4″-sulfonamidephenylazo)-3,6-disulfonaphthalene (RII): and 1,8-dihydroxy-2-(4′-chloro-2′-phosphonophenylazo)-7-(p-hippuric acid azo)-3,6-disulfonaphthalene (RIII). Loss of absorbance of three colour reagents at maximum absorption wavelengths is proportional to the concentration of chromium (VI) in solution. We have made use of the decolorization reactions between chromium (VI) and three colour reagents to determine chromium in steel by flow injection analysis, and relative error in sample determination is less than 5.0%. Response is linear from 0.84 to 6.72 μg/mL and optimum measuring acidity is 1.3–1.7 mol/L H2SO4 in three systems. The effect of interference ions on determination has been studied. 相似文献