• Title/Summary/Keyword: $^{13}C-NMR$ 분석

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Studies of Oxo-Nitrosyl Complexes(Ⅱ) Synthesis and Properties of Tungsten Oxo-Nitrosyl Complexes with Butylamidoxime Derivatives (산소-니트로실 착물의 연구 (제2보) 부틸아미드옥심 유도체의 텅스텐 산소-니트로실 착물의 합성과 특성)

  • Roh, Soo Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.39 no.11
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    • pp.856-862
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    • 1995
  • The tungsten oxo-nitrosyl complexes (n-Bu4N)2[W5O12(NO)2{RC(NH2)NHO}2{RC(NH)NO}2] (R=(CH3)2CH, CH3CH2CH2, CH3SCH2) have been synthesized by the reactions of polyoxotungsten complex (n-Bu4N)2[W6O19] and tungsten dinitrosyl monomeric complex [W(NO)2(acac)(CH3CN)2](BF4) with butylamidoxime derivatives. The prepared complexes have been characterized by elemental analysis, infrared, UV-visible, 1H NMR and 13C NMR spectroscopy. The pentanuclear species was formed by the interaction of the electron-withdrawing {W(NO)2}2+ unit between the two dinuclear tungsten {W2O5}2+ cores. We can estimate to exist large proton interactions viewed from the four doublet in 1H NMR spectrum of (n-Bu4N)2[W5O12(NO)2{(CH3)2CHC(NH2)NHO}2{(CH3)2CHC(NH)NO}2]. We also drew informations of the two different coordination mode and symmetry of the complexes because two ligands appear in 13C NMR spectra instead of four. The {W(NO)2}2+ unit has been cis-form and C2v symmetry in geometric structure.

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The Structure Analysis and Biosynthesis of $\beta$-glucan by Alcaligenes faecalis (Alcaligenes faecalis에 의한 $\beta$-glucan의 생합성과 구조 분석)

  • Ryu, Kang;Lee, Ki-Young;Lee, Eun-Kyu
    • KSBB Journal
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    • v.16 no.4
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    • pp.409-414
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    • 2001
  • Biosynthesis of curdlan( ${\beta}$-1,3 glucan) was shown by fluorscence on cellufluor medium. The highest production of curdlan was produced when glucose was used as a carbon source and ($NH_4$)$_2$$SO_4$ was used as a nitrogen source. ${\beta}$ -form of curdlan was detected in the fingerprint region (890 $cm^{-1}$) by FT-IR spectrum and shown homogeneous ${\beta}$ -1,3 glucan by $^{13}C$ NMR spectrum ($C_1$-103 ppm, $C_2$-73.2 ppm, $C_3$-86.4 ppm, $C_4$-68.7 ppm, $C^{5}$-76.63 ppm, $C_{6}$-61.2 ppm). Transition of structure from triple helix coil form to random coil form was appeared at 0.1 ∼0.25 M NaOH concentration. It was shown that natural curdlan is a triple helix form in neutral but becomes weak in alkaline condition.

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Synthesis and Characterization of Palladium (IV) Complexes with Guanine, Adenine, and Uracil Base (Guanine, Adenine 및 Uracil 염기를 갖는 팔라듐 (IV) 착물의 합성과 그 성질)

  • Oh Sang Oh;Chung Duck Young;Kim Hee Seon
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.679-684
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    • 1992
  • New Pd(IV) complexes have been prepared through the reactions of $trans-[Pd(en)_2Cl_2](ClO_4)_2 $(en = ethylenediamine) with Guanine, Adenine, or Uracil anion as purine and pyrimidine base. We identified the ratio of central metal versus ligands by $C{\cdot}H{\cdot}N$ elemental analysis and proposed the coordinating site of the base by infrared spectrum, $^1H-NMR,\; and\; ^{13}C$-NMR spectrum. Guanine or Adenine ligand coordinated at N7 site and an en ligand exchanged for $ClO_4^-$ counter ions of the starting material . As these results, the complexes showed the formula $[Pd(en)L_2(ClO_4)_2](ClO_4)_2{\cdot}(en)$, (L = Guanine, Adenine). But in the Uracil complex no exchange of the en ligand and $ClO_4^-$ occured and Uracil anion preferred the N1 to N3 as coordinating site, the complex $[Pd(en)_2(Urac)_2](ClO_4)_2(Urac = Uracil anion).$

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Characteristics of Ring-Opening Isomerization Polymerization of [4.3.0] Cyclic Pseudoureas ([4.3.0] 환상 유사 우레아의 이성화 개환중합과 특성평가)

  • Lee, Chan-Woo;Chung, Jin-Do
    • Polymer(Korea)
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    • v.35 no.4
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    • pp.308-313
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    • 2011
  • The ring-opening isomerization polymerization behavior of 2,5,6,7-tetrahydro-3H-imidazo[2,1-b] [1,3] oxazine(TII) has been studied under various conditions. The present study aimed at improving the low polymerizability of the above monomer (six-membered ring) up to a level comparable to that of 2,5,6-tetrahydroimidazo[2,1-b] [l,3] oxazole(TIO) (five-membered ring). The optimum result could be observed when methyl trifluoromethanesulfonate(MeOTf) and nitrobenzene were used as an initiator and a solvent in the polymerization at $60^{\circ}C$ for 24 h. Polymers were confirmed by$^1H$ NMR과$^{13}C$ NMR, and m measurements. The molecular weight obtained by gel permeation chromatography (GPC) corresponded to the molecular weight theoretically calculated from the feed ratio. The melting temperature ($T_m$) of TII was conspicuously different from that of TIO, because of the difference in the alkyl group.

Spectroscopic Analysis of the Ethanol + Methane Hydrate (에탄올+메탄 하이드레이트에 대한 분광학적 분석연구)

  • Lee, Jong-Won;Kang, Seong-Pil
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.146.2-146.2
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    • 2011
  • Molecular behaviors and crystal structures of the binary hydrates of $CH_4$ and ethanol were identified by means of 13C solid-state NMR and powder XRD methods at various concentrations of ethanol. In addition, NMR peak areas were used to calculate cage occupancies for both guest species. Obtained results showed that more $CH_4$ molecules are captured into hydrate phase per unit mass of ethanol molecules because $CH_4$ molecule can occupy sII large cages more, and pure $CH_4$ hydrate can form more as well at lower ethanol concentrations. Even though tuning phenomenon was already reported for some aqueous hydrate promoters such as THF, aqueous ethanol solutions are found to play the same tuning role in the binary clathrate hydrates in this study.

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Isolation of 3,4-Dihydroxybenzoic Acid, Which Exhibits Antimicrobial Activity, from Fruits of Gardenia jasminoides Ellis (치자 열매에서 항미생물 활성을 갖는 3,4-Dihydroxybenzoic Acid의 분리)

  • Yim, Cheol-Keun;Moon, Jae-Hak;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1386-1391
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    • 1999
  • The methanol extract of Gardenia jasminoides Ellis showed antimicrobial activity against bacteria and yeasts. The extract was successively purified with solvent fractionation, silica gel adsorption column chromatography, Sephadex LH-20 column chromatography, octadecylsilane column chromatography. The purified active substance was isolated by high performance liquid chromatography. The isolated compound was 3,4-dihydroxybenzoic acid which was determined by mass spectrometer, gas chromatograph-mass spectrometer, $^{1}H-nuclear$ magnetic resonance, $^{13}C-nuclear$ magnetic resonance and two-dimensional nuclear magnetic resonance. The content of 3,4-dihydroxybenzoic acid was $32.7\;{\mu}g/g$ in dried fruits of Gardenia jasminoides Ellis.

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Synthesis and Spectroscopic Studies of Metal Complexes Formed in the Reaction of Metal Ions with Urea at High Temperature (높은 온도에서 Urea와 금속이온과의 반응으로 얻어진 금속 Complexes의 합성과 분광학적 연구)

  • Gaballa, Akmal S.;Teleb, Said M.;Nour, El-Metwally
    • Journal of the Korean Chemical Society
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    • v.51 no.4
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    • pp.339-345
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    • 2007
  • Urea reacts with PtCl2, H2[PtCl6]·6H2O, H2[IrCl6] and Ni(CH3CO2)2 in aqueous solution at high temperature (60-80 °C) yielding [PtCl2(Urea)]·2H2O (1), (NH4)2[PtCl6] (2), (NH4)2[IrCl6]·H2O (3) and [Ni2(OH)2(NCO)2(H2O)2] (4) complexes, respectively. In complex 1, urea coordinates to Pt(II) as a neutral bidentate ligand via amido nitrogen atoms. In complexes 2, 3 and 4 it seems that the coordinated urea molecules decompose during the reaction at high temperature and a variety of reaction products are obtained. All complexes were isolated in moderate yields as dark green (1), yellow (2), pale brown (3) and faint green (4) precipitates, respectively. The reaction products were characterized by their microanalysis, IR, 1H and 13C NMR spectra as well as thermal analysis. General mechanisms describing the formation of these complexes were suggested.

Novel Synthesis of bis Acetylated Hybrid Pyrazoles as Potent Anticandidiasis Agents (항칸다디아 활성이 우수한 bis acetylated hybrid pyrazoles의 합성 연구)

  • Kanagarajan, V.;Ezhilarasi, M. R.;Gopalakrishnan, M.
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.256-261
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    • 2011
  • A new series of bis acetylated hybrid pyrazoles were synthesized and characterized by their melting point, elemental analysis, MS, FT-IR, one-dimensional $^1H$, and $^{13}C$ NMR spectroscopic data. All the synthesized compounds were tested for their in vitro antifungal activities against Candida sp. namely Candida albicans, Candida glabrata, Candida parapsilosis, Candida dubliniensis and Candida tropicalis. A close inspection of the in vitro anticandidal activity profile in differently electron donating ($CH_3$ and $OCH_3$) and electron withdrawing (-F, -Cl, and Br) functional group substituted phenyl rings of novel hybrid pyrazoles exerted strong anticandidal activity against all the tested Candida species.

Synthesis and Characterization of Poly(ethylene oxide) Derivatives Containing Carbonate Linkages (고분자 주사슬에 카보네이트 관능기가 도입된 새로운 폴리에틸렌 옥사이드 유도체의 합성 및 분석)

  • 최유선;차국찬;서정인;정동준;안정호
    • Polymer(Korea)
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    • v.25 no.6
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    • pp.759-764
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    • 2001
  • In order to obtain PEO with reduced crystallinity, novel PEO derivatives containing carbonate linkages in the main chain have been synthesized by the reaction of various molecular weight poly (ethylene glycol)s (PEGs) with dimethyl carbonate (DMC) in the presence of $H_2SO_4$ to yield methyl carbonate terminated PEGs, followed by condensation reaction under vacuum in the presence of titanium isopropoxide (TiP) catalyst. The number average molecular weight of PEGs used was in the range of 200 and 600 g/mol. The structure and compositions of the resulting polymers were characterized by $^1$H-NMR and $^{13}C-NMR$. Their thermal behavior and molecular weight were characterized by DSC/TGA and GPC, respectively.

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Extractives from Epimedium koreanum Nakai (삼지구엽초(Epimedium koreanum Nakai)의 추출성분)

  • Lee, Tae-Seong;Cho, Jae-Hyun;Hwang, Byung-Ho
    • Journal of Korea Foresty Energy
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    • v.24 no.2
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    • pp.16-23
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    • 2005
  • The air dried of Epimedium koreanum Nakai was extracted with MeOH and its extractives were concentrated with a vacuum evaporator. The extractives were fractionated with a series of n-hexane, chloroform (${CHCl}_3$), butanol (BuOH), ethyl acetate (EtOAc) and water on a separately funnel. Each fraction was freeze dried to give some dark brown powder. The EtOAc and BuOH soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-n-hexane mixture as eluents. The isolated compounds were tested with a cellulose TLC developed with TBA and 6% acetic acid and then visualized on UV lamp or sprayed with vanillin-HCl-EtOH. The purified compounds were flavonoids and their glycosides, and organic acid as follows : (+)-catechin, icariin, hyperoside, Ikarisoside A and caffeic acid. The structures of each compounds were confirmed by $^1H-NMR,\;^{13}C-NMR$ and Mass spectra. Also, executed qualitative analysis as use GC/MS(Libraries search) about ${CHCl}_3$ soluble compounds of each part.

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