二环己基并18冠6的制备方法

二苯并-18－冠-6;二环己基并18冠6的制备方法     

过渡金属与新型硝基酚臂式氮杂18-冠-6配位性能的研究

合成并表征了1,10-二氧-4,7,13,16-四氮杂18-冠-6 (1)母体及其四取代硝基酚臂式衍生物 (2)。在H₂O-DMSO(V/V=1/4)混合溶剂中用UV-Vis光谱法对冠醚2与H⁺、Mn²⁺、Co²⁺、Ni²⁺、Cu²⁺、Zn²⁺、Cd²⁺和Hg^{2+相似文献}   

Competitive Potentiometric Study of the Thermodynamics of Complexation of Some Transition and Heavy Metal Ions with Dibenzopyridino-18-crown-6 in Methanol using Ag+ Ion as a Probe

The complexation of dibenzopyridino-18-crown-6 with some transition and heavy metal ions in methanol solution at various temperatures was studied by a competitive potentiometric method using a Ag⁺/Agelectrode system. The stoichiometry and stability of the resulting complexes were computed by the MINIQUAD program. The stability of the resulting complexes varied in the order Ag⁺ > Pb²⁺ > Tl⁺ > Cu²⁺ > Cd²⁺ > Zn²⁺. The enthalpy and entropy of the resulting 1:1 complexeswere evaluated from the temperature dependence of the stability constants.The complexes of all cations were enthalpy-stabilized but entropy-destabilized,except for Ag⁺ and Pb²⁺ ions,which were also entropy-stabilized.     

Synthesis and characterization of new polymeric phthalocyanines substituted with diaza-18-crown-6 macrocycles through ethyleneoxy bridges

A tetranitrile monomer was synthesized by nucleophilic aromatic substitution of N,N′-bis(2-hydroxyethyl)-4,13-diaza-18-crown-6 onto 4-nitrophthalonitrile. A series of polymeric metal-free and metallophthalocyanine (M = 2H, Zn, Cu, Co and Ni) polymers was prepared by polymeric tetramerization reaction of the tetranitrile monomer with proper materials. The electrical conductivities of the polymeric phthalocyanines measured as gold sandwiches were found to be ∼10⁻⁹–10⁻⁴ S cm⁻¹ in a vacuum and in argon. The extraction ability of the metal-free polymeric phthalocyanine was evaluated in tetrahydrofuran using several alkali metal picrates such as Li⁺, Na⁺, K⁺ and Cs⁺. The extraction affinity of the metal-free polymeric phthalocyanine for K⁺ was found to be highest in the heterogeneous solid–liquid phase extraction experiments. The disaggregation property of the metal-free polymeric phthalocyanine was investigated with sodium, potassium and ammonium ions and methanol. All the novel compounds were characterized by using elemental analysis, UV–Vis, FT-IR, NMR and MS spectral data and DTA/TG.     

On the solid-state conformations of 18-crown-6 complexes

A procedure for displaying macrocylic torsion angles as a map on polar coordinates is discussed with reference to the solid-state conformations of l8-crown-6 and its complexes. The maps aid in comparisons of related structures, in the perception of pseudo-symmetry elements, and in the classification of the conformations of 18-crown-6. Only four conformational groups are found in the 1 : 1 complexes of 18-crown-6 with sodium, potassium, rubidium, cesium, thallium(I), calcium and strontium cations. The relationship of donor number, mean cavity radius and effective ionic radius combined with skeletal drawings of the donors and the polar map of the torsion angles provide a composite picture of the structures and insight into the balance between cation-donor interaction energy and conformational energy.This paper is dedicated to the memory of the late Dr C. J. Pedersen.     

Crystal structure of supramolecular complexes formed by 18-crown-6 andcis-anti-cis-dicyclohexano-18-crown-6 (host) with 3,4-diaminofurazane (guest)

An X-ray—diffraction study is reported for two molecular complexes containing 3,4-diamino-1,2,5-oxadiazole as guest (G) with 18-crown-6 (18-C-6) andcis-anti-cis-dicyclohexano-18-crown-6 (DCH-6B) as host. Both complexes are of the polymeric-chain structure with the guest molecule bridging two crown neighbours. ComplexI: [18-C-6*G*H₂O], 111, monoclinic,P2₁/n,a=8.171(1),b=15.042(2),c=16.209(6) Å, =101.15(2)°, finalR-factor 0.068. ComplexII: [DCH-6B*G], 11, monoclinicC2/c,a=21.212(4),b=9.380(2),c=13.049(3) Å, =108.61(3)°, finalR 0.047.     

Second crystal modification of 1,10-diazonia-18-crown-6 dichloride

The second crystal modification (II) of 1,10-diazonia-18-crown-6 dichloride [H₂DA18C6]²⁺·2Cl^?, where [H₂DA18C6]²⁺ is the 1,10-diaza-18-crown-6 dication (DA18C6) with two protonated nitrogen atoms, was investigated by XRD. The monoclinic modification (II) (space group P2₁/n, a = 9.600 Å, b = 5.689 Å, c = 15.749 Å, β = 91.03°, Z = 2) was solved by direct methods and refined by full-matrix least squares analysis in an anisotropic approximation to R = 0.032 for all 2494 independent reflections collected (CAD-4 automatic diffractometer, λMoK _α). In modification II, the conformation of the DA18C6 dication and the ion packing differ from those in triclinic modification I investigated previously.     

Dibenzo-18-crown-6 modified with kojic acid fragments

Diazonium salts were prepared by diazotization of 4′-amino-, 4′,4″-, and 4′,5″-diaminodibenzo-18-crown-6. Their coupling products with kojic acid (5-hydroxy-2-hydroxymethyl-γ-pyrone) were synthesized for the first time: 4′-(6-aza-5-hydroxy-2-hydroxymethyl-γ-pyronyl)-, 4′,4″-di-(6-aza-5-hydroxy-2-hydroxymethyl-γ-pyronyl)-, and 4′,5″-di-(6-aza-5-hydroxy-2-hydroxymethyl-γ-pyronyl)-dibenzo-18-crown-6. __________ Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 415–416, September–October, 2006.     

微波辅助二苯并-18-冠-6的合成

以邻苯二酚与二甘醇二取代物为原料,氢氧化钾为碱和模板剂,在微波辅助下,采用“一锅煮”法合成二苯并-18-冠-6。 经单因素及正交实验考察了原料、溶剂、时间、温度和功率对反应收率的影响,获得了最佳的工艺条件：以邻苯二酚与二氯乙醚为原料,二甲亚砜为溶剂,反应温度70 ℃,时间60 min,功率500 W,收率可达46.3%。     

吖啶基功能化二苯并-18-冠-6的合成

通过改变离去基团的活性、亲核试剂、溶剂的极性、离子性及反应温度等,对传统的U llm ann合成法进行了优化,将二苯并-18-冠-6进一步功能化,合成了未见文献报道的N,N′-二-(9-吖啶基)-4,4′-二氨基二苯并-18-冠-6,收率在87%以上。其结构经1H NMR,IR及元素分析表征。     

New Derivatives of Dibenzo-18-crown-6 with Salsolidine and Salsoline Fragments

New derivatives of dibenzo-18-crown-6 were prepared by condensing 4,4(5)-dibenzo-18-crown-6-dicarboxylic acid dichloride with salsolidine and salsoline. The structures of these compounds were proved by PMR and IR spectral methods.     

光敏离子载体丹磺酰基-单氮杂-18冠-6的合成和光谱性质

以丹磺酰氯（ＤＮＳ－Ｃｌ）为光敏元件,单氮杂冠醚为识别元件,合成,鉴定了题示光敏离子载体ＤＮＳ－ＭＡＣ（Ｏ５）,研究了它在水溶液和各种有机溶剂中的吸收光谱和发光光谱。对比ＤＮＳ－Ｃｌ,基于在不同极性溶剂中荧光光谱的变化,采用Ｓｏｌｖａｃｈｒｏｍｉｃ法,由Ｌｉｐｐｅｒｔ方程估算得它们的激发态偶极矩。     

Transmembrane potentials in systems containing 18-crown-6

Electric potentials of MK-40 cation-exchange membrane, which is immersed in aqueous solutions of KCl, RbCl, and macrocyclic polyether 18-crown-6, have been measured. The possibility of preliminary calculations of biionic and multiionic potentials from equilibrium constants of ionic exchange and electrochemical mobilities of cations in the sulfo cationite is demonstrated.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1489–1490, August, 1995.     

顺、反异构的二羟基二苯并-18-冠-6的方便合成

用顺、反二氨基二苯并－18－冠－6与氟硼酸和亚硝酸正戊酯反应制得相应的芳基重氮氟硼酸盐，经水解，以较好的收率制得了二羟基二苯并－18－冠－6，后者是合成功能高分了的有用单体。     

N-取代吩噻嗪和DDQ的电荷转移络合作用

具有盼嘤酸化学结构的化合物有广泛的用途I‘－＼其中吩嘤埃衍生物在医学上用作抗精神病药物特别受到药理学家们的注意，发现其药理作用与其分子提供电子的能力有关卜‘」但是我们应该注意到，作为抗精神病药物的吩嚷嚷衍生物，其吩座爆分子的氮原子都连有一个叔胺基链问，例如氯丙障（I）和奋乃静（11）．而我们知道，胺类特别是叔胺类有强的提供电子的能力＊；在上述的药物分子中是主要的提供电子因素，因此以这类化合物作为给体研究其供电子能力，是不能实际反映吩嘤嗓分子本身的给电子能力的．吩嘤噪类属于二苯并杂环化合物，分子中既…     

二苯并-18-冠-6与碱金属苦味酸盐在氯仿中的相互作用

研究一种方法以测定二苯并-18-冠-6在氯仿中与碱金属苦味酸盐相互作用的若干参数。这些参数是:络合物的无限稀释摩尔电导 A_0,络合物的解离常数 K_d(或 k_d),络合物中冠醚与盐的分子比,冠醚对苦味酸盐的络合常数 K_c(或 k_c),以及冠醚存在下苦味酸盐紧密离子对的饱和浓度[MA]等。     

Spectrophotometric Determination of Albendazole Drug in Tablets: Spectroscopic Characterization of the Charge-transfer Solid Complexes

Simple, rapid and reliable method for the determination of albendazole (ABZ) was described. This includes the utility of some Π‐acceptors such as 2,3‐dichloro‐5,6‐dicyano‐p‐benzoquinone (DDQ) and 3,6‐dichloro‐2,5‐dihy‐ droxy‐p‐benzoquinone (p‐CLA) for estimation of ABZ drug (act as donor). The experimental conditions were optimized and the system obeys Beer's law for 7.50–80 and 10.00–85.00 µg·mL^?1 of ABZ using DDQ and p‐CLA, respectively. The molar absorptivity and Sandell sensitivity were calculated to be 1.83×10³ and 1.12×10³ L·mol^?1·cm^?1, and 2.60 and 3.40 ng·cm^?2 using DDQ and p‐CLA, respectively. The limits of detection and quantification were calculated to be (7.42 and 6.73) and (9.94 and 4.13) µg·mL^?1 using DDQ and p‐CLA, respectively. The proposed methods were successfully applied to the determination of ABZ in commercially available dosage forms. The reliability of the assays was established by parallel determination by the official method and recovery studies. The chemical structures of the solid charge‐transfer (CT) complexes formed via reaction between ABZ under study and Π‐acceptors, have been elucidated using elemental analyses (C, H and N), IR, ¹H NMR and mass spectra.     

双环己基18冠6对水／硝基苯界面离子的促进传输

Li~-和H~-因较强的亲水性,较难穿越液/液界面进行传输。本文报道了冠醚双环已基18冠6对Li~+,Na~+,Rb~-和H~-在水/硝基苯界面的促进传输行为,求得了相应促进传输过程的一系列参数,并对被传输离子在传输过程中的形态变化进行了初步的探讨。     

Acylation of Dibenzo-18-crown-6 with Alkali-metal Acetates in Polyphosphoric Acid

The acylation of dibenzo-18-crown-6 by lithium, sodium, and potassium acetates in polyphosphoric acid was studied. Complexes of dibenzo-18-crown-6 with the acetates were obtained. A new method is proposed for the production of mono- and diacetyldibenzo-18-crown-6 by the reaction of dibenzo-18-crown-6 complexes with metal acetates in polyphosphoric acid. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1146–1149, August, 2005.     

Complex formation of Ag+ with polyether 18-crown-6

The complex formation of Ag⁺ with polyether 18-crown-6 (18C6) and their solvation have been studied using calorimetric and potentiometric methods in H₂O-EtOH solvents in wide range of ethanol concentration. The standard enthalpies of dissolution AgNO₃, AgClO₄ and 18C6 in aqueous-ethanol solvents are obtained. The stability of a complex [Ag18C6]⁺ grows with increasing the EtOH content a solvent. Using the method based on the thermodynamic characteristics of solvation of metal-ion, ligand and complex-ion the interpretation of the results has been given. This revised version was published online in August 2006 with corrections to the Cover Date.