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1.
A. N. Levov A. I. Komarov A. T. Soldatenkov G. V. Avramenko S. A. Soldatova V. N. Khrustalev 《Russian Journal of Organic Chemistry》2008,44(11):1665-1670
By condensation of cycloalkanes with 2-{2-[2-(2-formylphenoxy)ethoxy]ethoxy}benzaldehyde and ammonium acetate by Petrenko-Kritchenko method first representatives of new heterocyclic systems, bis(benzo)-aza-14-crown-4 ethers containing a 7-aza-bicyclo[3.3.1]nonane or its homologous fragment, were obtained in 6–15% yield. With growing cycle of the initial cycloketone the yield of the azacrownophane considerably grew. By means of XRD analysis the molecular structure was established of four synthesized macrocycles, the relative configuration of asymmetrical atoms was determined, and the size of the internal cavities of the azacrown part was estimated. 相似文献
2.
Bronislaw P. Czech Wolodymyr Zazulak Anand Kumar Uriel Olsher Hadar Feinberg Shmuel Cohen Gil Shoham N. Kent Dalley Richard A. Bartsch 《Journal of heterocyclic chemistry》1992,29(6):1389-1400
Seventeen new substituted 14-crown-4 derivatives 3-10, 35-40, 42, 45 and 46 are described. A series of nine compounds 2-10 with two, three or four substituents in the 6- and/or 13-positions was synthesized in good yields from the appropriate diols and ditosylates using improved cyclization conditions. The solid state structures of 6,6,13,13-tetra(benzyloxymethyl)-14-crown-4 ( 8 ) and lithium thiocyanate complexes of trans- and cis-6,13-bis(spiro-2,2-dichlorocyclopropyl)-14-crown-4 ( 45 ) and ( 46 ), respectively, have been determined. 相似文献
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Chyong Khong Khieu A. T. Soldatenkov An’ Le Tuan A. N. Levov A. F. Smol’yakov V. N. Khrustalev M. Yu. Antipin 《Russian Journal of Organic Chemistry》2011,47(5):766-770
By triple condensation of thiourea or guanidine with 1,ω-bis(2-formylphenoxy)-3-oxapentane and ammonium acetate first representatives
of the new class of ethers bis(benzo)aza-14-crown-4 were obtained in 28–73% yield that included as a subunit a symm-perhydrotriazine ring. This reaction also proceeds readily with N-monomethyl- and N-monopropenyl-substituted thioureas affording
the corresponding derivatives of triazinoazacrown ether. At the same time urea in the similar condensation does not form the
expected perhydrotriazinoazacrown ether. The molecular structure of one perhydroazacrown ether as a complex with a chloroform
molecule was established by XRD analysis. 相似文献
5.
The alkali metal/group 4 metal/polychalcogenides Cs(4)Ti(3)Se(13), Rb(4)Ti(3)S(14), Cs(4)Ti(3)S(14), Rb(4)Hf(3)S(14), Rb(4)Zr(3)Se(14), Cs(4)Zr(3)Se(14), and Cs(4)Hf(3)Se(14) have been synthesized by means of the reactive flux method at 823 or 873 K. Cs(4)Ti(3)Se(13) crystallizes in a new structure type in space group C(2)(2)-P2(1) with eight formula units in a monoclinic cell at T = 153 K of dimensions a = 10.2524(6) A, b = 32.468(2) A, c = 14.6747(8) A, beta = 100.008(1) degrees. Cs(4)Ti(3)Se(13) is composed of four independent one-dimensional [Ti(3)Se(13)(4-)] chains separated by Cs(+) cations. These chains adopt hexagonal closest packing along the [100] direction. The [Ti(3)Se(13)(4-)] chains are built from the face- and edge-sharing of pentagonal pyramids and pentagonal bipyramids. Formal oxidation states cannot be assigned in Cs(4)Ti(3)Se(13). The compounds Rb(4)Ti(3)S(14), Cs(4)Ti(3)S(14), Rb(4)Hf(3)S(14), Rb(4)Zr(3)Se(14), Cs(4)Zr(3)Se(14), and Cs(4)Hf(3)Se(14) crystallize in the K(4)Ti(3)S(14) structure type with four formula units in space group C(2)(h)()(6)-C2/c of the monoclinic system at T = 153 K in cells of dimensions a = 21.085(1) A, b = 8.1169(5) A, c = 13.1992(8) A, beta = 112.835(1) degrees for Rb(4)Ti(3)S(14);a = 21.329(3) A, b = 8.415(1) A, c = 13.678(2) A, beta = 113.801(2) degrees for Cs(4)Ti(3)S(14); a = 21.643(2) A, b = 8.1848(8) A, c = 13.331(1) A, beta = 111.762(2) degrees for Rb(4)Hf(3)S(14); a = 22.605(7) A, b = 8.552(3) A, c = 13.880(4) A, beta = 110.919(9) degrees for Rb(4)Zr(3)Se(14); a = 22.826(5) A, b = 8.841(2) A, c = 14.278(3) A, beta = 111.456(4) degrees for Cs(4)Zr(3)Se(14); and a = 22.758(5) A, b = 8.844(2) A, c = 14.276(3) A, beta = 111.88(3) degrees for Cs(4)Hf(3)Se(14). These A(4)M(3)Q(14) compounds (A = alkali metal; M = group 4 metal; Q = chalcogen) contain hexagonally closest-packed [M(3)Q(14)(4-)] chains that run in the [101] direction and are separated by A(+) cations. Each [M(3)Q(14)(4-)] chain is built from a [M(3)Q(14)] unit that consists of two MQ(7) pentagonal bipyramids or one distorted MQ(8) bicapped octahedron bonded together by edge- or face-sharing. Each [M(3)Q(14)] unit contains six Q(2)(2-) dimers, with Q-Q distances in the normal single-bond range 2.0616(9)-2.095(2) A for S-S and 2.367(1)-2.391(2) A for Se-Se. The A(4)M(3)Q(14) compounds can be formulated as (A(+))(4)(M(4+))(3)(Q(2)(2-))(6)(Q(2-))(2). 相似文献
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1-Acetoxyethyl 2-(2-fluoro-4-biphenylyl) [14C-methyl]propionate (14C-Me-FP 83), a novel nonsteroidal antiinflammatory agent for injection, was synthesized in order to investigate the metabolic fate. 14C-Me-FP 83 was obtained by the condensation of 2-(2-fluoro-4-biphenylyl) [14C-methyl]propionic acid with 1-chloroethyl acetate. The chemical yield of 1 was 62% after purification. The specific activity was 258 kBq/mg (6.99 microCi/mg) and its radiochemical purity was 99% in thin layer chromatographic method. 相似文献
8.
Compounds [Rb(18-crown-6)]4As14.6NH3 (1) and [Li(NH3)4]4P14.NH3 (2) were prepared by the reaction of Rb4As6 with SbPh3 and 18-crown-6 and by the reduction of white phosphorus with elemental lithium in liquid ammonia, respectively. Both were characterized by low-temperature single-crystal X-ray structure analysis. They were found to contain the Ci symmetrical Pn14(4-) anion (Pn = P, As), which consists of two nortricyclane-like Pn7-cages connected by a single bond. Molecular complexes of [Rb(18-crown-6)(NH3)]2[Rb(18-crown-6)]2As14 are formed in 1, which are connected to fanfold sheets via N-H...O bonds. The anion is isolated in 2, and N-H...N bonds result in the formation of {[Li(NH3)4](mu-NH3)2[Li(NH3)4]}2+ cationic complexes. 相似文献
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通过Sonogashira偶联等反应,合成了三嵌段化合物9,10-双-(对-(甲氧基二缩三乙二醇基)苯基乙炔基)蒽,通过1H NMR和基质辅助激光解吸电离时间飞行质谱(MALDI-TOF-MS)对其结构进行了表征。利用差示扫描量热仪(DSC)、偏光显微镜(POM)及小角X射线散射仪(SAXS)等技术手段对其本体自组装行为进行了研究,结果表明,化合物在固态相自组装成近晶A相(SmA相)。光谱分析表明,该化合物继承了二取代蒽类发光材料具有高荧光量子产率(Φf)的特点,是一种性能良好的光致发光材料。 相似文献
11.
Benzyl-14C-1-[bis(4-fluorophenyl)methyl]-4-(2,3,4-trimethoxybenzyl) piperazine dihydrochloride (14C-KB-2796), a new cerebral vasodilator, was synthesized in order to investigate the metabolic fate. The synthesis of carboxy-14C-2,3,4-trimethoxybenzoic acid (IV) was accomplished by the reaction of 2,3,4-trimethoxybromobenzene (II) with ter-butyllithium followed by carboxylation with 14C-carbon dioxide generated from 14C-barium carbonate. Formyl-14C-2,3,4-trimethoxybenzaldehyde (VI) was prepared by the reduction of the methyl ester of IV. The free base of 14C-KB-2796 was obtained by the condensation of VI with bis(4-fluorophenyl)methyl-piperazine, and converted to I. An overall radiochemical yield from 14C-barium carbonate was 39%, the specific activity was 1,816.7 MBq/mmol (49.1 mCi/mmol) and its radiochemical purity was 99% in reverse isotope dilution analysis and thin layer chromatographic method. 相似文献
12.
A new series of 4-substituted derivatives of dibenzo-14-crown-4 including 4-nitro-DB14-crown-4 ( 2a ), 4-bromo-DB14-crown-4 ( 2b ), 4-chloro-DB14-crown-4 ( 2c ) and 4-formyl-DB14-crown-4 ( 2d ) has been synthesized with and without a lithium cation template. No matter with or without the template, a satisfactory correlation between the nature of the substituent group on the benzene ring and the reaction yield is observed. The larger σ values for the substituent groups gave lower yields. 相似文献
13.
Chromogenic benzo-12-crown-4, benzo-13-crown-4 and benzo-14-crown-4 ethers have been compared with monoaza-12-crown-4 and monoazal-13-crown-4 ethers. Of these compounds, monoaza-13-crown-4 exhibited the best analytical characteristics toward the selective determination of lithium. K(ex)Li/K(ex)Na was 525 for the monoaza-crown-4 compound. 相似文献
14.
Junwu Chen Kevin Ka‐Leung Cheuk Ben Zhong Tang 《Journal of polymer science. Part A, Polymer chemistry》2006,44(3):1153-1167
A group of new amphiphilic poly(phenylacetylene)s bearing polar oligo(ethylene oxide) pendants, poly{4‐[2‐(2‐hydroxyethoxy)ethoxy]phenylacetylene} ( 1 ), poly(4‐{2‐[2‐(2‐hydroxyethoxy)‐ethoxy]ethoxy}phenylacetylene) ( 2p ), poly(3‐{2‐[2‐(2‐hydroxyethoxy)ethoxy]ethoxy}phenylacetylene) ( 2m ), poly(4‐{2‐[2‐(2‐methanesulfonyloxyethoxy)ethoxy]ethoxy}phenylacetylene) ( 3 ), poly(4‐{2‐[2‐(p‐toluenesulfonyloxyethoxy)ethoxy]ethoxy}phenylacetylene) ( 4 ), poly(4‐{2‐[2‐(2‐trimethylsilyloxy‐ethoxy)ethoxy] ethoxy}phenylacetylene) ( 5 ), and poly(4‐{2‐[2‐(2‐chloroethoxy)ethoxy]ethoxy}phenylacetylene) ( 6 ), were synthesized with organorhodium complexes as the polymerization catalysts. The structures and properties of the polymers were characterized with IR, UV, NMR, and thermogravimetric analysis. 1 , 2p , and 2m , the three polymers containing pendants with hydroxyl groups, were oligomeric or insoluble. The organorhodium complexes worked well for the polymerization of the monomers without hydroxyl groups, giving soluble polymers 3 – 6 with a weight‐average molecular weight up to ~160 × 103 and a yield up to 99%. Z‐rich polymers 3 – 6 could be prepared by judicious selections of the catalyst under optimal conditions. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 1153–1167, 2006 相似文献
15.
Ribot F Martinez-Ferrero E Boubekeur K Hendrickx PM Martins JC Van Lokeren L Willem R Biesemans M 《Inorganic chemistry》2008,47(13):5831-5840
A tin(IV) oxoalkoxo cluster with unprecedented architecture has been prepared and characterized by single-crystal X-ray diffraction. The cluster obeys the formula Sn 12O 8(OH) 4(OEt) 28(HOEt) 4 (1) and is based on an elongated centrosymmetric assembly of 12 six-coordinate tin centers, 28 peripheral ethoxy groups (terminal and bridging), 8 oxo bridges (mu2 and mu3), 4 hydroxy bridges (mu2), and 4 ethanol molecules that are all bound to tin atoms and interact strongly, through hydrogen bonds, with an ethoxy group located on a vicinal tin atom. This compound has also been fully characterized in solution by multinuclear 1D and 2D NMR, with all of its (119)Sn, (1)H, and (13)C NMR resonances assigned with respect to the structure. Altogether, the data allowed unambiguous location of the hydroxy groups. Information on the exchange of the ethoxy groups is also presented. 相似文献
16.
A series of neutral ionophore-based lithium-selective liquid-membrane electrodes have been prepared and the electrode performance compared with similar electrodes based on the lithium ionophores ETH 1810-ortho-nitrophenyl octyl ether (oNPOE) and ETH 2137-bis(1-butylpentyl) adipate (BBPA). By using a diamide substituted 14-crown-4 macrocycle, selectivities for Li+ in the presence of Na+ of log kpotLi,Na = -3.25 and -2.92 were obtained for diisobutylamide-oNPOE and di-n-butylamide-oNPOE derivatives. The di-n-butylamide-oNPOE based electrode functioned satisfactorily in serum, exhibiting a fast response time (10-15 s), an acceptable lifetime of 50 d and minimal protein interference. 相似文献
17.
L. L. Dmitrieva L. P. Nikitina A. I. Albanov N. A. Nedolya 《Russian Journal of Organic Chemistry》2005,41(11):1583-1593
Reaction of 2-[2-(vinyloxy)ethoxy]methyl- and 2-(allyloxymethyl)oxiranes with 2-propynyl- and phenylethynylmagnesium bromides (10–55°C, 0.5–4 h) resulted in new representatives of the series of 1-organyloxy-5-hexyn-2-ols, -5-phenyl-4-pentyn-2-ols, and -3-bromo-2-propanols in 50–99% yields. During distillation the 1-[2(vinyloxy)ethoxy]-5-phenyl-4-pentyn-2-ol and -3-bromo-2-propanol transform respectively into 2-methyl-4-(3-phenyl-2-propynyl)- and 2-methyl-4-(bromomethyl)-1,3,6-trioxocanes via intramolecular cyclization involving the hydroxy and vinyloxy groups. 相似文献
18.
A. N. Levov Tuan Le An’ A. I. Komarova V. M. Strokina A. T. Soldatenkov V. N. Khrustalev 《Russian Journal of Organic Chemistry》2008,44(3):456-461
The condensation of dialkyl ketones with α,ω-bis(2-formylphenoxy)- or α,ω-bis(1-formylnaphthalen-2-yloxy)-3-oxapentane and-3,6-dioxaoctane in the presence of ammonium acetate according to Petrenko-Kritchenko gave 14–41% of new bis(areno) aza crowns, bis(areno)piperidinoaza-14-crown-4 and bis(benzo)-piperidinoaza-17-crown-5, having functional substituents in the piperidine fragment. The yield of the aza crown ether appreciably decreases upon extension of the polyether chain in the aldehyde component. The molecular structure of two of the obtained macrocyclic compounds and the relative configuration of asymmetric carbon atoms in the piperidine ring were determined by X-ray analysis, and the size of their internal cavities was estimated. 相似文献
19.
Masoumeh Hasani Mojtaba Shamsipur 《Journal of inclusion phenomena and macrocyclic chemistry》2004,48(3-4):135-139
Interactions of hexaaza-18-crown-6 (HA18C6) and tetraaza-14-crown-4 (TA14C4) with iodine have been investigated spectrophotometrically in chloroform solution. The observed time dependence of the charge-transfer band and subsequent formation of I3 - in solution were related to the slow transformation of the initially formed 1:1 macrocycle. I2 outer complex to an inner electron donor-acceptor (EDA) complex, followed by fast reaction of the inner complex with iodine to form a triiodide ion, as follows: macrocycle + I2→fast K f macrocycle.I2 (outer complex) macrocycle.I2 (outer complex) →slow (macrocycle.I+)I- (inner complex) macrocycle.I+)I- (inner complex) + I2→slow (macrocycle.I+)I3 -. The pseudo-first-order rate constants at various temperatures for thetransformation process were evaluated from the absorbance-time data. The activation parameters (Ea, Δ H?, and Δ S?) for thetransformation were obtained from the temperature dependence of the rate constants. The stoichiometry and formation constants of the resulting EDA complexes have also been determined. It was found that the (TA14C4.I+)I3 - is more stable the (HA18C6.I+)I3 - complex in chloroform solution. 相似文献
20.
The synthesis of the novel asymmetric ligand 1-[bis(2-pyridylmethyl)amino]-3-[2-(2-pyridyl)ethoxy]-2-hydroxypropane (ppepOH) is reported. The ligand is suitable to form asymmetric dinuclear complexes with various transition metal ions. As an example, the synthesis and X-ray structure analysis of the dinickel(II) complex [Ni(2)(ppepO)(C(6)H(5)COO)(2)(CH(3)COOH)]ClO(4).C(4)H(10)O are described. The complex crystallizes in the monoclinic space group P2(1)/n with the following unit cell parameters: a = 13.704(10) ?, b = 14.849(10) ?, c = 22.697(14) ?, beta = 96.80(5) degrees, Z = 4. The nickel(II) ions are bridged by the alkoxy donor of the ligand and two benzoate anions. The hexadentate ligand leaves a free coordination site at one of the nickel(II) ions, which is occupied by a monodentate coordinated acetic acid molecule. The coordination of the neutral acetic acid molecule is selectively stabilized by a strong intramolecular hydrogen bond of the acidic proton to the &mgr;-alkoxo bridge of the dinuclear complex. The asymmetric complex was prepared in order to mimic the substrate uptake in the dinuclear active site of ureases. The magnetic and spectroscopic properties of the complex were determined and related to those of the urease enzymes. 相似文献