• Title/Summary/Keyword: 1H-NMR spectroscopy

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Interactions and Ionic Conductivities of Poly(epichlorohydrin) Graft Copolymer Electrolyte Membranes (Poly(epichlorohydrin) 가지형 공중합체 전해질막의 상호작용 및 이온 전도도)

  • Koh, Joo-Hwan;Lee, Kyung-Ju;Park, Jung-Tae;Ahn, Sung-Hoon;Kim, Jong-Hak
    • Membrane Journal
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    • v.20 no.3
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    • pp.203-209
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    • 2010
  • Amphiphilic graft copolymers based on poly(epichlorohydrine) (PECH) were synthesized using atom transfer radical polymerization (ATRP). Successful graft polymerization of poly(methyl methacrylate)(PMMA) and poly(butyl methacrylate) (PBMA) from PECH was confirmed by nuclear magnetic resonance ($^1H$ NMR) and FT-IR spectroscopy. Upon the introduction of KI or LiI to the graft copolymers, the ether stretching bands were shifted to a lower wavenumber due to coordinative interactions. Ionic conductivities of PECH-g-PBMA complexes were always higher than those of PECH-g-PMMA complexes, resulting from higher mobility of rubbery PBMA chains. The maximum ionic conductivity of $2.7{\times}10^{-5}\;S/cm$ was obtained at 10 wt% of KI for PECH-g-PBMA electrolytes.

Synthesis of Low Molecular-weight Poly (Propylene Carbonate)-Poly (Ethylene Glycol) Block Copolymers through $CO_2$/Propylene Oxide Copolymerization (이산화탄소/프로필렌 옥사이드 공중합을 통한 저분자량 폴리(프로필렌 카보네이트)-폴리(에틸렌 글리콜) 블록 공중합체의 합성)

  • Lee, Sang-Hwan;Cyriac, Anish;Jeon, Jong-Yeob;Lee, Bun-Yeoul
    • Clean Technology
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    • v.17 no.3
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    • pp.244-249
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    • 2011
  • We synthesized low molecular-weight polymers bearing hydrophobic and hydrophilic parts in a chain through $CO_2$/propylene oxide copolymerization. When hydrophilic poly (ethylene glycol) bearing -OH group (s) at the end group (s) was added as a chain transfer agent in the $CO_2$/propylene oxide copolymerization catalyzed by a highly active catalyst, block polymers were formed. If poly (ethylene glycol) (PEG) bearing -OH group only at an end was fed, PEG-block-PPC diblock copolymer was obtained. When PEG bearing -OH group at both ends was fed, PPC-block-PEG-block-PPC triblock copolymer was obtained. We confirmed formation of block copolymers by $^1H$-NMR spectroscopy and GPC studies.

Composition and Structure Confirmation of Glucitol Fatty Acid Polyesters (Glucitol Fatty Acid Polyesters의 조성 및 구조확인)

  • Chung, Ha-Yull;Yoon, Hee-Nam;Kong, Un-Young;Kim, Jung-Han
    • Korean Journal of Food Science and Technology
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    • v.25 no.2
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    • pp.148-153
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    • 1993
  • Composition and structure of synthetic glucitol fatty acid polyesters (GPE)-a potential fat substitute-were investigated. Also degree of substitution (D.S) of GPE was determined according to the relative ester distribution within it to evaluate the feasibility of GPE using as a fat substitute. The GPE was separated into single ester group by a normal-phase HPLC and D.S of it was identified to be 6. Absorption band at $1747\;cm^{-1}$ in the IR spectrum of GPE indicated that there were ester bonds within GPE molecules. which link fatty acid moiety to glucitol. Disappearance of the hydroxyl proton signals of glucitol in the H-NMR spectrum of GPE implied that most of hydroxyl groups in glucitol participated in the formation of ester bonds with fatty acids. In addition the D.S estimated from the quantitative proton integration of GPE coincided well with the D.S of GPE determined by hydroxyl value measurement. In conclusion, the GPE synthesized in this study was found to be a glucitol fatty acid hexaester so that it is expected to be used as a fat substitute in the near future.

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Investigation of Isomerism in Anthracene-Isothiouronium Salts and Application of these Salts for Anion Sensing

  • Nguyen, Quynh Pham Bao;Kim, Jae-Nyoung;Kim, Taek-Hyeon
    • Bulletin of the Korean Chemical Society
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    • v.30 no.9
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    • pp.2093-2097
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    • 2009
  • Novel fluorescent anion chemosensors based on anthracene-isothiouronium derivatives were synthesized. Isomerism due to the intramolecular mobility in these isothiouronium salts was detected by $^1H$ NMR spectroscopy. The effect of the substituent, temperature and solvent on the isomerism was also examined. The anthracene-isothiouronium sensor showed significant fluorescent enhancement upon the addition of various anions such as fluoride, acetate, and dihydrogen phosphate, even in the presence of water.

Lipoxygenase Inhibitor from Defatted Nutmeg Seed

  • Kim, Hyo-Jin;Chung, Shin-Kyo;Park, Sang-Won
    • Preventive Nutrition and Food Science
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    • v.3 no.3
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    • pp.216-220
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    • 1998
  • Lipoxygenase inhibitory acitivity of the methanolic extract of 60 different kinds of plant seeds was determined by a spectrophotometric method using a soybean lipoxigenase(SLO) and linolenic acid. Among the extracts examined, the methanolic extract of nutmeg(Myristical fragrans)seed showed the most potent SLO inhibitory activity. To isolate SLO inhibitor, hence, the defatted methanol extract was further partitioned with ether, ehtylacetate , and n-butanol , stepwise. The ether souble fraction was successively chromatographed on silica gel, Sephadex LH-20 and preparative TLC. Three phenolic compounds were isolated , and one of them showing a strong SLO inhibition activity was identified as a 2,6-dihydroxy-9-(3', 4', -dihydroxyphenyl)nonylphenone (IC50a=0.39$\mu\textrm{g}$/ml) by 1H-& 13C0NMR, IR, and MS spectroscopy.

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Poly(methyl methacrylate-co-styrene)/Silicate Nanocomposites Synthesized by Multistep Emulsion Polymerization

  • Park, Yeong-Suk;Kim, Yoon-Kyung;Chung, In-Jae
    • Macromolecular Research
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    • v.11 no.6
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    • pp.418-424
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    • 2003
  • Exfoliated poly(methyl methacrylate-co-styrene) [P(MMA-co-ST)]/silicate nanocomposites were synthesized through a multistep emulsion polymerization. The methyl methacrylate monomers were polymerized first and then the styrene monomers were polymerized. The nanocomposites had core-shell structures consisting of PMMA (core) and PS (shell); these structures were confirmed by $^1$H NMR spectroscopy and TEM, respectively. P(MMA-co-ST) copolymers showed two molecular weight profiles and two glass transition temperatures (T$_{g}$) in GPC and DMA measurements. At 30 $^{\circ}C$, the nanocomposites exhibited 83 and 91 % increases in their storage moduli relative to the neat copolymer because the silicate layers were dispersed uniformly in the polymer matrix.x.

Synthesis of 2'-Hydroxydihydrochalcone from Flavone

  • Kim, Mi-Hyang;Shin, Bok-Kyu;Won, Dong-Ho;Han, Jae-Hong
    • Journal of Applied Biological Chemistry
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    • v.50 no.2
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    • pp.85-87
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    • 2007
  • To establish the synthetic method for dihydrochalcones as an important bioactive compounds, 2'-hydroxydihydrochalcone has been synthesized from the reduction of flavone in 20% yield. Flavone with five equivalents of ammonium formate in the presence of Pd/C in methanol under $N_2$ atmosphere produced the C-ring opened product. It was characterized by UV-VIS, ESI-MS and $^1H-NMR$ spectroscopy, and identified as 2'-hydroxydihydrochalcone.

Synthesis and Antifungal Activities of Some Aryl (3-Methyl-Benzofuran-2-yl) Ketoximes

  • Benkli, Kadriye;Gundogdu-Karaburun, Nalan;Karaburun, Ahmet-Cagrl;Ucucu, Umit;Demirayak, Seref;Kiraz, Nuri
    • Archives of Pharmacal Research
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    • v.26 no.3
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    • pp.202-206
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    • 2003
  • In this study, some aryl (3-methyl-benzofuran-2-yl) ketoximes and their ethers and esters were synthesised. The structure elucidation of the compounds was performed by IR, $^1H-NMR$, MASS spectroscopy and elemental analyses. Antifungal activities of the compounds were examined and moderate activity was obtained.

Isolation and Identification of an Unauthorized Tadalafil Analogue in a Commercial Functional Food (시판 기능성식품으로부터의 타다라필 유도체 부정첨가물질의 분리 및 구조규명)

  • Baek, Du-Jong
    • YAKHAK HOEJI
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    • v.54 no.4
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    • pp.240-243
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    • 2010
  • High-performance liquid chromatography (HPLC) screening method revealed that a propolis product marketed as a functional food contained an undeclared substance similar to tadalafil, the active ingredient of the prescription drug Cialis$^{(R)}$ approved for the treatment of male erectile dysfunction. In order to identify the illegal additive, the propolis product was extracted with methylene chloride, and the extract was purified further using semipreparative HPLC. The chemical structure of the isolated substance was elucidated based on IR, LC/MS-ESI, and $^1H$- and $^{13}C$-NMR spectroscopy, which showed the characteristics similar to tadalafil. The only difference was the substitution of the methyl group at the piperazinedione ring of tadalafil to the amino group of the identified illegal additive.

Synthesis of Norbornene Block Copolymers Containing Polyhedral Oligomeric Silsesquioxane by Sequential Ring-Opening Metathesis Polymerization

  • Kwon Young-Hwan;Kim Kyung-Hoe
    • Macromolecular Research
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    • v.14 no.4
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    • pp.424-429
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    • 2006
  • The synthesis of a series of poly(POSS-NBE-b-MTD) copolymers was successfully accomplished, taking advantage of sequential, ring-opening, metathesis block copolymerization using $RuCl_2(=CHPh)(PCy_3)_2$ catalyst. By using cyclopentyl-POSS-norbornene (POSS-NBE) monomer as the first block in the block copolymer, living poly(POSS-NBE) with controlled molecular weight and narrow molecular weight distribution was produced. Then, poly(POSS-NBE-b-MTD) copolymers were successfully prepared, in which sequential monomer addition of methyltetracyclododecene (MTD) to the living poly(POSS-NBE) chain ends was utilized to achieve quantitative crossover efficiency. Characterization by $^1H$ NMR spectroscopy and GPC confirmed the high definition and structural integrity of the poly(PO$S-NBE-b-MTD) copolymers. Thermal properties-and morphologies of the POSS-containing block copolymer nanocomposites were also investigated by using thermogravimetric analysis (TGA), transmission electron microscopy (TEM), and wide-angle X-ray scattering (WAXS).