• Title/Summary/Keyword: IR and C-13 NMR spectra

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Synthesis of Polymeric Thiazolidinediones and L-Ascorbic Acid Towards the Development of Insulin-Sensitizer

  • Lee Sun Mi;Jeon Raok
    • Archives of Pharmacal Research
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    • v.28 no.4
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    • pp.377-381
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    • 2005
  • Polymers, containing 5-(4-O-methylacryloylbenzyl)thiazolidine-2,4-dione [MABTZD]; poly (MABTZD), poly(MABTZD-co-AA) and poly(MABTZD-co-AMAA), were prepared, and identified by FT-IR, $^1H-$ and $^{13}C-NMR$ spectra. The MABTZD unit contents in poly(MABTZD-co-AA) and poly(MABZD-co-AMAA) were 11.3 and $27.7 mol\%$, respectively. The number average molecular weights of the polymers, as determined by GPC, ranged from 16,800 to 22,300, and with polydispersity indices of $1.2\sim1.4$.

Iridoid Glycoside (IV) -Studies on the Iridoid Glucoside of Melampyrum roseum Max- (Iridoid 배당체(配糖體) (IV) -꽃며느리밥풀의 Iridoid 배당체(配糖體)에 관(關)한 연구(硏究)-)

  • Chung, Bo-Sup;Kim, Young-Ho
    • Korean Journal of Pharmacognosy
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    • v.13 no.3
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    • pp.106-111
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    • 1982
  • Melampyrum roseum Max. is an annual herb in Scrophulariaceae plants. The materials were collected in Kyeongi-Do in 1980. The BuOH extract was evaporated under reduced pressure. The residue was column chromatographed over silica gel with benzene-MeOH (8 : 1) as an eluent and it gave the amorphus powder. Compound I has a molecular formula $C_{17}H_{26}O_{10}$ and it was identified as mussaenoside by chemical data, UV, IR, NMR spectra and compared with the authentic sample of mussaenoside tetraacetate.

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Differences in Structural Characteristics and Eu(III) Complexation for Molecular Size Fractionated Humic Acid (분자량별 분류에 따른 휴믹산의 구조적 특성 및 Eu(III)과의 착물 반응 특성 비교에 대한 연구)

  • Shin, Hyun-Sang;Rhee, Dong-Seok;Kang, Kihoon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.159-166
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    • 2001
  • A humic acid(HA, Aldrich Co) sample was subjected to ultrafiltration for molecular size fractionation and three fractions of different nominal size($F_1$: 1,000-10,000 daltons; $F_2$: 10,000-50,000 daltons; $F_3$: 100,000-300,000 daltons) were obtained. The structural characteristics of the size-fractionated HA were analyzed using their IR and solid state C-13 NMR spectral data, and the carboxylate group contents of the humic acids were determined using their pH titration data. The $^7F_0-{^5}D_0$ excitation spectra of Eu(III) complexes of the size-fractionated mgHA in aqueous solution were acquired($[Eu(III)]=1.0{\times}10^{-4}mol\;L^{-1}$, $(HA)=470-970mg\;L^{-1}$) at pH 5.0 using a pulsed tunable laser system, in which metal binding properties of the size-fractionated HA were elucidated and compared on another. Characterization of the IR and C-13 NMR spectral data indicated that the fraction($F_3$) with molecules of larger size were primarily aliphatic, while the fractions($F_1$, $F_2$) with smaller molecules of less than 50,000 daltons were predominantly aromatic. Titration data were consistent with an increase in the number of carboxylate groups per unit mass as molecular size became smaller. The $^7F_0-{^5}D_0$ excitation spectral data of Eu(III)-humate complexes showed that the peak maxima on these spectra were shifted toward lower energies with increasing molecular size of HA, indicating the higher degree of bindings of the Eu in the molecules of larger size. We also discussed the relationship of the lower energy shifts of the maximum peaks with increasing the molecular size of HA with the structural differences of the size-fractionated HA.

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Analysis of ${\beta}-(1{\to}3)(1{\to}6)-Glucan$ Produced by Aureobasidium pullulans IMS-822 (Aureobasidium pullulans IMS-822가 생산하는 ${\beta}-(1{\to}3)(1{\to}6)-Glucan$의 특성 분석)

  • Lee, Seog-June;Ahn, Keug-Hyun;Park, Chan-Sun;Yoon, Byung-Dae;Kim, Min-Soo
    • Korean Journal of Microbiology
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    • v.45 no.1
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    • pp.63-68
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    • 2009
  • The exo-polysaccharide producing microorganism, Aureobasidium pullulans IMS-822, was isolated and identified from soil. The viscosity-average molecular weight of exo-polysaccharide was calculated as $8.9{\times}10^5$ by Mark-Houwink equation. The sugar component of exo-polysaccharide was determined as glucose by HPLC analysis. The IR spectra indicated that the exo-polysaccharide has an absorption peak at 890 $cm^{-1}$ for the ${\beta}-configuration$ of D-glucan. The $^{13}C$ NMR signal at ${\delta}$ 86.62 ppm arose from the substituted C-3 of glucose. The signal at ${\delta}$ 72.11 ppm was assigned to C-6 of branched ${\beta}-(1{\to}3)-D-glucosyl$ residues. Viscosity and Congo red reaction indicated that {\beta}-(1{\to}3)(1{\to}6)-glucan$ produced by A. pullulans IMS-822 has a highly ordered hydrogen-bond dependent conformation in aqueous solution, which collapses in strong alkaline solution.

Structural Characteristics of the Water Soluble Browning Reeaction Products Isolated from Korean Red Ginseng (홍삼으로부터 분리한 수용성 갈변물질의 구조 특성)

  • 이종원;고학룡;심기환
    • The Korean Journal of Food And Nutrition
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    • v.11 no.5
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    • pp.499-505
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    • 1998
  • The purpose of this study was to ivestigate the structural characteristics of waste soulble browning reaction prodcuts (WS-BRPs) isolated from Korean red ginseng. They all showed the maximum absorbances at near 280 nm. Their IR spectra suggested the presence of hydroxyl, amide carbonyl and aliphatic methine groups. From sugar analysis it was identified that L and S-1 contained two kinds of suggar, glucose and xylose, and S-2, a fructose together with glucose and xylose. Thirteen different amino acids were identified in L. Ten amino acids from S-1 and seven amino acids from S-2 were identified using Auto Amino Acid Analyzer. Glycine, serine and glutamic acid in S-1 and one unknown amino acid and glycine in S-2 were detected as the major amino acids, respectively. From the 1H-and 13C-NMR spectra, it was identified that a number of sugar moieties, carbonyl and carbon double bonds (only in S-2) were contained in the three WS-BRP components. Approximate number of sugar moiety of L, S-1 and S-2 was determined to be 8∼10, 9∼11 and 4∼5, respectively. Contents of nitrogen, carbon and hydrogen showed L>S-1>S-2.

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Nucleophilic Addition Reaction of Thioglycolic acid to 2-Fluorenylidene chalcone Derivatives (2-Fluorenylidene chalcone유도체에 대한 Thioglycolic acid의 친핵성 첨가 반응에 관한 연구)

  • Lee, Ki-Chang;Lee, Kwang-Il;Hwang, Yong-Hyun;Ryu, Jung-Wook;Yoon, Cheol-Hun
    • Journal of the Korean Applied Science and Technology
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    • v.13 no.1
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    • pp.107-113
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    • 1996
  • Fluorenylidene chalcone derivatives were synthesized by condensation. The structure of these compounds were ascertained by means of UV, melting point, IR and $^1H-NMR$ spectra. The nucleophilic addition reaction kinetics of Thioglycolic acid to fluorenylidene chalcone was investigate by UV in 20% $dioxane-H_2O$ at $25^{\circ}C$. The rate equation which were applied over a wide $pH1.0{\sim}13.0$ range. On the basis of general base catalysis and confirmation of addition reaction product, the nucleophilic addtion reaction kinetics of thioglycolic acid to fluorenylidene chalcone were measured by the pH change. From the result of the above caption, a plausible nucleophilic addition reaction mechanism of thioglycolic acid to fluorenylidene chalcone was proposed. These compounds may be used as the starting materials for the preparation of the engineering plastics or the germicide.

Purification and Identification of Phenol Compounds with Inhibitory Activity on Helicobacter pylori from Rhododendron mucronulatum Flos. Extracts (진달래꽃(Rhododendron mucronulatum Flos.) 추출물로부터 Helicobacter pylori 억제 효과를 가지는 phenol성 물질의 정제 및 동정)

  • Ju, In-Sik;Cho, Young-Je
    • Journal of Life Science
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    • v.19 no.8
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    • pp.1125-1131
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    • 2009
  • The antimicrobial activities of Helicobacter pylori as a functional food source with water and 60% ethanol extracts from Rododendron mucronulatum Turcz. flowers were examined. The total phenol content of 60% ethanol extracts (30.6${\pm}$0.14 mg/g) from Rododendron mucronulatum Turcz. flowers was higher than that of water extracts (23.2${\pm}$0.21 mg/g). The inhibitory activities of Rododendron mucronulatum Turcz. extracts on H. pylori was determined to clear zone of 15 mm in 80% ethanol extracts. Purification of inhibitory compounds was carried out in Sephadex LH-20 and MCI-gel CHP-20 column chromatography using a gradient procedure, with increasing ethanol(0${\rightarrow}$100%) in $H_2O$. The chemical structure of the purified inhibitory compounds of H. pylori was identified to be quercitrin (quercetin-3-O- rhamnopyranoside), myricitrin (myricetin-3-O-rhamnopyranoside), quercetin by FAB-MS, NMR and IR spectra.

Synthesis, Spectral and Thermal Studies of Lanthanide(III) Complexes of Phenylbutazone (Phenylbutazone의 란탄(III) 착물에 대한 합성, 스펙트럼 및 열적 연구)

  • Anoop, M.R.;Binil, P.S.;Jisha, K.R.;Suma, S.;Sudarsanakumar, M.R.
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.612-619
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    • 2011
  • Lanthanide(III) complexes of 1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB) have been synthesized and characterized by elemental analyses, molar conductance measurements, IR, UV-Vis. and NMR spectra. The spectral data reveal that the PB acts as a bidentate and mono-ionic ligand coordinating through both the carbonyl oxygens of the pyrazolidinedione ring. The molar conductance data suggest that the complexes are non-electrolytes. The thermal behaviour of the complexes was studied by TG and DTG in air atmosphere and the results provide information about dehydration, thermal stability and thermal decomposition. The final products are found to be the corresponding metal oxides. The thermodynamic parameters and kinetic parameters were evaluated for the dehydration and decomposition stages. The negative entropy values of the decomposition stages indicate that the activated complexes have a more ordered structure than the reactants and that the reactions are slower than normal. Based on these studies, the complexes have been formulated as $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La and Ce) and $[Ln(PB)_3(H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd and Sm).

A Study on the Nucleophilic Addition Reaction of L-cysteine for PVS (PVS 유도체에 대한 L-Cysteine의 친핵성 첨가반응에 관한 연구)

  • Lee, Ki-Chang;Lee, Kwang-Iil;Yoon, Chul-Hun;Hwang, Sung-Kwy;Kong, Seung-Dae
    • Journal of the Korean Applied Science and Technology
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    • v.12 no.2
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    • pp.99-105
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    • 1995
  • Phenylvinylsulfone derivatives were synthesized by Kirners condition. The structure of these compounds were ascertained by means of ultraviolet, melting point, IR and $^1H-NMR$ spectra. The nucleophilic addtion reaction kinetics of L-cysteiene for phenylvinylsulfone was investigated by ultraviolet spectrophotometery in 40% $EtOH-H_2O$ at $25^{\circ}C$. The rate equations which were applied over a wide pH $1.0{\sim}13.0$ range. On the basis of general base catalysis and confirmation of addtion reaction product, the nucleophilic addtion reaction kinetics of L-cysteiene for phenylvinylsulfone were measured by the pH change. From the result of the above caption, a plausible nucleophilic addtion reaction mechanism of L-cysteiene for phenylvinylsulfone was proposed. These compounds may by used ad the starting materials for the preparation of the engineering plastics or the germicide.

Study on the Improved Abrasion Resistance of Polycarbonate Substrate by UV-curable Organic/Inorganic Hybrid Coatings (자외선 경화형 유기/무기 복합코팅에 의한 폴리카보네이트의 내마모성 향상 연구)

  • 윤석은;우희권;김동표
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.389-398
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    • 2000
  • Transparent, abrasion resistant coatings with 4~13 ${\mu}{\textrm}{m}$ thickness were prepared by spin-coating on polycarbonates with organic/inorganic hybrid solutions, followed by UV curing and heat treatment at 12$0^{\circ}C$ for 12 hours. The coating solutions were composed of inorganic phase and organic phase in 0:100, 20:80, 30:70, 50:50, 80:20 wt% ratios, respectively, mixed with photoinitiator, senaitizer and surfactant. The inorganic phase was formed by sol-gel reaction of TEOS and silane coupling agent MPTMS in 1 : 2 or 2 : 1 molar ratios, the organic phase consisted of difunctional urethane acrylate oligomeric resin, multifunctional acrylate TMPTA and HDDA in 4 : 3 : 3 wt% ratio. The coating systems were investigated by FT-IR, $^{29}$ Si-NMR spectra. In addition, TGA/DSC for thermal analysis and SEM, AFM observation for coated surface were examined. Gererally, the homogeneity of phases, the surface smoothness of coating and abrasion resistance were improved with the higher content of inorganic component. Namely, coating system with below 10 $\AA$ surface roughness and T$_{g}$ of 15$0^{\circ}C$ showed only 10% decrease in light transmittance after abrasion test, whereas uncoated polycarbonate substrate exhibited 46% decrease..

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