• Title/Summary/Keyword: 핵자기 공명

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Alcohol-Amine Synergism in the Organic Solvent Extraction of Tungsten (텅스텐의 아민용매 추출과정에서의 알코올의 작용)

  • Lee Hoosung;Uh, Young Sun;Sohn, Youn Soo
    • Journal of the Korean Chemical Society
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    • v.16 no.6
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    • pp.361-368
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    • 1972
  • The organic solvent mixture of 5 % trioctylamine and 5 % n-octyl alcohol in n-hexane could be loaded with tungsten to 62 g $WO_3$/1 whereas the amine alone could be loaded only to 37 g $WO_3$/1. Molecular interaction between amine and tungstate ion during the solvent extraction process and the synergistic effect of alcohol in enhancing the solubility of the amine-tungstate complex have been studied by NMR spectroscopy. Tungsten has been shown to be extracted as a polymeric tungstate ion into the organic phase to form a trioctyl ammonium polytungstate salt, which was more stabilized in the hydrocarbon medium by interacting with alcohol via hydrogen bonding between the tungstate ion and alcohol.

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A Study on the Nuclear Magnetic Resonance Spectra of Halogen Substituted Anisole Derivatives (할로겐 치환아니솔유도체의 핵자기공명스펙트라에 관한 연구)

  • You Sun Kim
    • Journal of the Korean Chemical Society
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    • v.21 no.2
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    • pp.94-101
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    • 1977
  • The NMR spectra of 2,4-disubstituted or 2,4,6-trisubstituted anisole derivative were examined to study the chemical shift of the ring proton signal. It was found that the chemical shift of the ring proton nearest to the 2-substituted group was influenced by the deshielding effect of the neighboring substituted groups in order of the Van der Waals radii of those groups. These observations were interpreted as a steric influence of 2-substituted group on the reactivity of the neighboring ring proton itself. The spectroscopical data were presented and the results were discussed with views of the above conceptions.

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Synthesis and Characterization of Molybdenum Complexes with Schiff Bases (I). Bis-(N-aryl salicylaldiminato) of dioxomolybdenum (VI) Complexes (몰리브덴의 시프-염기착물의 합성과 그 성질 (제1보). 다이옥소 몰리브데늄(VI)의 아릴살릴실알디미나토착물)

  • Oh Sang Oh;Bon Kweon Koo
    • Journal of the Korean Chemical Society
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    • v.29 no.3
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    • pp.226-232
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    • 1985
  • Dioxomolybdenum(VI) complexes, MoO$_2$(H-Sal-R)$_2$, R; arylamines, have been synthesized by reactions of dioxobis (salicylaldehydato) molybdenum(VI) with various primary amines. These complexes have been characterized by electric conductivity and spectroscopic studies. Infrared, uv-vis, and proton nmr spectra show that the complexes are six-coordinated with cis-MoO$_2$ group. And mass spectra indicates that the combining ratios for Mo (VI)-ligand are 1 : 2. They are yellow, stable for a considerably long time in the atmosphere at room temperature and slightly soluble in alcohol, dichloromethane and dimethylformamide but insoluble in benzene, ether and carbon tetrachloride.

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Characterization of Hyaluronic Acid Membrane Cross-linked with Lactide (락타이드로 가교시킨 히아루론산 막의 특성)

  • Kwon, Ji-Young;Cheong, Seong-Ihl
    • Polymer(Korea)
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    • v.29 no.6
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    • pp.599-604
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    • 2005
  • The hyaluronic acid (HA) with excellent biocompatibility has been combined with lactide, the ester dimer of polylactide, with good biodegradability to produce biocompatible materials which can control the period of degradation in a human body. By freeze frying method, HA and lactide were crosslinked with crosslinking agent, 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC). Degree of lactide and EDC reaction was determined by the analysis of nuclear magnetic resonance spectroscopy. Both lactyl group and EDC conversion increased as the mole ratio of lactide to HA increased from 5 to 13. The membrane swelled less and became more brittle with the more addition of lactyl group resulting from the higher mole ratio of lactide to HA. Swelling ratio decreased and tensile modulus increased due to the more addition of lactyl group as the EDC concentration increased or reaction temperature decreased. Drug release experiment from various membranes with different degree of crosslinking showed that permeability decreased with increasing degree of crosslinking. The degradation became slower with the more addition of lactyl group. Mechanical property and degradation rate of the synthesized membrane were shown to be controlled through adjusting operation parameters such as mole ratio, temperature, and crosslinking agent concentration.

Characterization of Lactide/Hyaluronic Acid Polymer Cross-Linked by 1,3-Butadiene Diepoxide (1,3-Butadiene Diepoxide에 의해 가교된 락타이드/히아루론산 고분자의 특성)

  • Han, Gwang-Seon;Bae, Jung-Eun;Kim, In-Seop;Cheong, Seong-Ihl
    • Polymer(Korea)
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    • v.32 no.4
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    • pp.390-396
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    • 2008
  • The hyaluronic acid (HA) polymers cross-linked with lactide (LA) using the crosslinking agent, 1,3-butadiene diepoxide (BD), were prepared in order to develop a biomedical material for tissue engineering. The degree of lactide and BD reaction of the crosslinked polymer was determined by the analysis of nuclear magnetic resonance spectroscopy. Both degree of reaction and swelling ratio increased with BD concentration or LA/HA mole ratio. Tensile modulus decreased with increasing BD concentration or decreasing LA/HA mole ratio. Degradation was shown to be progressed at two different stages and became slow with increasing BD concentration. It was shown that the first stage degradation was mainly due to the decomposition of ester linkage in the crosslinked structure. The cell growth inhibition increased with BD concentration. Although cytotoxicity was slightly observed in the high BD concentration, the value was very low (below 6%) enough not to affect the cell growth.

A Study on the Rearrangement of 1,3-Thiazolidine Sulfoxides to Dihydro-1,4-thiazines (1,3-티아졸리딘술폭시드의 디히드로-1,4-티아진 유도체로의 전위에 관한 연구)

  • Wha Suk Lee;Hoh Gyu Hahn;He-Duck Mah
    • Journal of the Korean Chemical Society
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    • v.33 no.2
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    • pp.247-256
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    • 1989
  • 4-Acetyl-5,6-dihydro-2-methyl-1,4-thiazine carboxylic acid derivatives 24 were prepared by ring expansion of corresponding thiazolidine sulfoxides. Oxidation of 2-methyl-1,3-thiazolidine-2-acetic acid derivatives 12 gave a mixture of cis and trans sulfoxides, 14 and 15. Assignments of the cis and trans sulfoxides were based on the $^1HNMR$ and IR spectroscopy and regioselectivity of deuterium exchange reaction. With PTSA as acid catalyst both the cis and trans sulfoxide, 14 and 15 were transformed via sulfenic acid 18 to dihydro-1,4-thiazine 24. However, under the neutral conditions (in DMF at $100^{\circ}C$) the trans sulfoxides 15 rearranged via sulfenic acid 21 to isomeric dihydrothiazines 27. The mechanism of formations of 24 and 27 is also discussed.

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Synthesis and Characterization of Dinuclear Mo(Ⅲ) and V(Ⅲ) Complexes (Ⅴ) (몰리브덴(Ⅲ)과 바나듐(Ⅲ) 이핵 착물의 합성과 특성 (제5보))

  • Oh, Sang-Oh;Lyou, Eun-Young
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.530-537
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    • 1995
  • The neutral complexes $MCl_3(phda)(MeCN)]$ and $[MCl_3(PPh_3)_2(MeCN)]$ (M=Mo, V) were prepared by the reaction of $MCl_z$, (M=Mo; z=5, M=V; z=3) with N, P-donating ligands in acetonitrile solution. Addition of AgClO_4$ to these neutral monomeric complexes in acetone solution afforded $MCl_{3-n}L_2(MeCN)(S)_n](ClO_4)_n$ (n=1, 2 : s=solvent). Two types of asymmetrical homo- and hetero-dinuclear complexes have been synthesized. The type of chloride bridged dinuclear complex is $[(MeCN)(phda)ClM({\mu}-Cl)_2M'Cl(PPh_3)_2(MeCN)](ClO_4)_2.$ And the type of pyrazine bridged complex is $[(MeCN)(phda)Cl_2M({\mu}-pyz)M'Cl_2(PPh_3)_2(MeCN)](ClO_4)_2.$ These complexes were characterized by elemental analysis, $^1H,\;^13C$ NMR, IR, Far-IR and UV-Vis spectroscopy.

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Synthesis and Characterization of Homo-, Hetero-Dinuclear Mo(Ⅲ) and V(Ⅲ) Complexes (Ⅳ) (몰리브덴(Ⅲ) 과 바나듐(Ⅲ) 호모 및 헤테로 이핵 착물의 합성과 특성 (제 4 보))

  • O, Sang O;Yu, Eun Yeong
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.808-818
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    • 1994
  • The neutral compounds [$MCl_3L_2$(MeCN)] (M = Mo, V: L = $PPh_3$, 1/2 phda) have been prepared from the reaction of starting material $MCl_z$ (M = Mo; z = 5, M = V; z = 3) with N,P-donating ligands in acetonitrile solution. Addition of $AgClO_4$ to these neutral monomeric compounds in acetone solution were produced [$MCl_3-_nL_2(MeCN)(S)_n$]$(ClO_4)_n$ (n = 1, 2 : s = solvent). Finally treatment of bivalent cationic compound and neutral compound was formed chloride bridged dinuclear complex $[(MeCN)(L)_2ClM({\mu}-Cl)_2M'Cl(L)_2(MeCN)](ClO_4)_2$ and treatment of univalent cationic compound with half equivalent pyrazine to pyrazine bridged complex $[(MeCN)(L)_2Cl_2M({\mu}-pyz)M'Cl_2(L)_2(MeCN)](ClO_4)_2$. These complexes are characterized by elemental analysis, $^1H$, $^{13}C$ NMR, IR, Far-IR and UV-Vis spectroscopy.

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Study on Structure of 9-Barbaralyl Cation by 1$^{13}C$ NMR Chemical Shift (탄소-13 핵자기공명 화학적 이동을 이용한 9-바바라릴 양이온의 구조에 관한 연구)

  • Jung-Hyu Shin;Yang-Soo Ahn
    • Journal of the Korean Chemical Society
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    • v.31 no.2
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    • pp.190-196
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    • 1987
  • The structure of 9-barbaralyl cation was examined by Hammett-Brown plot using $^{13}C$ NMR chemical shifts. 9-Aryltricylclo$[3.3.1.0^{2,8}]$]nonan-9-yl cation (5) and 9-aryltricyclo-$[3.3.1.0^{2,8}]$nona-3,6-dien-9-yl cation (6) were prepared from the corresponding carbinols in $FSO_3H-SO_2ClF$ solution at -$120^{\circ}C$, and their chemical shifts of cation centers were measured. The slopes, ${\rho}^{C+}$ values, of the Hammett-Brown plot of (5) and (6) were -5.01 and -7.52, respectively. From these values themselves, it seemed that the double bonds participated in the delocalization of the positive charge. However, comparing ${\rho}^{C+}$ value and ${\rho}^{C_a^+}$ value in 9-barbaralyl cation (6) and those in 8,9-dehydroadamantyl cation (7), we concluded that 9-barbaralyl should be represented by the structure 4 shown in Scheme I.

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Stability Constants for Transition Metal ions of Hexadentate $N_6$ Ligands Containing Two Pyridyl Groups (피리딘을 포함하는 여섯자리 $N_6$ 리간드와 전이금속 이온 착물의 안정도상수)

  • Kim, Sun-Deuk;Kim, Jun-Kwang;Park, Yoon-Yul
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.397-402
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    • 1999
  • The open-chain hexadentate $N_6$, ligand containing two pyridyl groups, 1,15-bis(2-pyridyl)-2,6,10,14-tetraazapentadecane (bpyped) has been synthesized as its tetrahydroehloride salt and characterized by EA, IR, NMR, and Mass. Its proton dissociation constants($logK{^n}_H$) and stability constants ($log\;K_{ML}$) for Co(II), Ni(II), Cu(II) and Zn(II) ions were determined at $25^{\circ}C$ and ionic strength 0.10 M($KNO_3$) in aqueous solution by potentiometry and compared with those or analogous $N_6$ ligands contain one or two propylenic spacers, which make six-membered chelate rings, between the aliphatic nitrogen atoms.

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