• Title/Summary/Keyword: Carbon 13 NMR

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Correlation of Chemical Shifts with Substituent Parameters in N-Benzyl Derivatives of Pyrrole,3a,7a-Dihydroindole,and Indole Esters

  • Jeon, Kyu-Ok;Yu, Sook-Yu;Lee, Chang-Kiu
    • Bulletin of the Korean Chemical Society
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    • v.23 no.9
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    • pp.1241-1255
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    • 2002
  • Series of m- and p-substituted benzyl derivatives of pyrrole, tetramethyl 1-benzyl-3a,7a-dihydroindole-2,3,3a,4-tetracarboxylate, and trimethyl 1-benzylindole-2,3,4-tricarboxylate were prepared and their 13C NMR spectra were obtained in 0.1 M solutions of chloroform-d. Both single substituent parameter and dual substituent parameter analyses were carried out to correlate the substituent chemical shifts. The ${\beta}$ carbon of the indole series showed the most profound substituent effect dependence as well as the best correlation. The results are explained by the hyperconjugation of the benzyl methylene group.

Production of Inulin fructotransferase(depolumerizing)by Arthrobacter sp. A-6 (Arthrobacter sp. A-6에 의한 Inulin Fructotransferase (depolymerizing)의 생산)

  • 박정복;권영만;최용진
    • Microbiology and Biotechnology Letters
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    • v.23 no.1
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    • pp.68-74
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    • 1995
  • A bacterial strain A-6 producing the high level of an extracellular inulin fructotransfe rase(depolymerizing)(EC 2.4.1.93) which converts inulin into di-D-fructofuranose dianhydride III (DFAIII) was isolated from soil. The isolated strain could be classified as a species belonging to the genus Arthrobacter based on its morphological and physiological characteristics identified in this work. Production of the enzyme was induced by inulin, and the highest activity was detected in the slightly acidic medium supplemented with 2.5% inulin and 0.1% trypton as a sole carbon and a nitrogen source, respectively. Under the optimal conditions, the enzyme activity in the culture supernatant reached approximately 60 uints/ml after 96 hours of cultivation. The optimum pH and temperature for the crude enzyme preparation from Arthrobacter sp. A-6 were pH 5.0 and 60$\circ$C , respectively. The DFA produced by the action of the inulin fructotransferase was confirmed to be DFAIII by paper chromatography, HPLC and $^{13}$C-NMR spectroscopy.

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Characterization of microbial poly-$\beta$-hydroxybutyrate (Microbial Poly-$\beta$-hydroxybutyrate의 구조특성)

  • Moon Sik Kim;Jong Kun Lee;Sang Joon Lee;Soo Min Park
    • Textile Coloration and Finishing
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    • v.7 no.1
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    • pp.51-57
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    • 1995
  • Poly-$\beta$-hydroxybutyrate(PHB) was biosynthesized using Alcaligenes sp. FL-027. Alcaligenes sp. FL-027 was cultivated by fed-batch methods, in order to promote cell growth and PHB accumulation with carbon source. The cells were first grown at 3$0^{\circ}C$ on the fermentor. The structure of biosynthesized PHB is investigated by the NMR, IR. The crystalline portions were identified through the use of DSC and X-ray diffractometer. The melting point was about 16$0^{\circ}C$ and the diffraction peaks of (020) and (110) were shown at 13$^{\circ}$ and 17$^{\circ}$, respectively.

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An Analytical Method for the Validation of a Salt-enhancing Peptide Using a Liquid Chromatography and a Nuclear Magnetic Resonance (NMR) Spectroscopy (HPLC와 NMR를 이용한 염미성 펩타이드 분석방법 검증)

  • Park, Sun You;Jeong, Yong Jin;Kim, Mi-Yeon;Hwang, Ji Hong;Kwon, Taeg Kyu;Seo, Young Ho
    • Journal of Life Science
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    • v.27 no.11
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    • pp.1324-1330
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    • 2017
  • Salt, or sodium chloride (NaCl), is a critical ingredient in many foods. It has roles in the flavor profiles of food products, textures of foods and preservation of foods against microbes. However, it increases risks of hypertension and is closely related to the development of cardiovascular disease. In recent years, health concerns related to sodium intake caused an increased demand for salt-reduced products in worldwide; it became necessary to develop natural salt-alternative products that are globally competitive. In a recent study, researchers succeeded in obtaining a natural salt enhancer through the hydrolysis of vegetable- and animal-matter mixtures. This study used various methods to identify and quantify peptide-containing arginine as a salt-alternative peptide (SAP) in an optimum combination. Arginine, or dipeptide-containing arginine, was analyzed as a standard substance using an NMR spectroscopy. The NMR carbon signal of the guanidine group of the standard substance was verified in a similar location (the L-arginine (Arg) was 156.8 ppm, the Arg-Alanine was 156.4 ppm and the Arg-Serine was 156.4 ppm). The results suggested that it is possible to analyze peptide-containing arginine quantitatively through the hydrolysis of vegetable- and animal-matter mixtures.

Structures and some Properties of the Antimicrobial Compounds in the Red Alga, Symphyocladia latiuscula (참보라색우무에서 추출한 항균물질의 구조 및 특성)

  • LIM Chi-Won;LEE Jong-Soo;CHO Young-Je
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.33 no.4
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    • pp.280-287
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    • 2000
  • Three antimicrobial compounds (SL-l, SL-2 and SL-3) were isolated and identified from the marine red alga, Symphyocladia latiuscula. In addition, their biological functionalities such as cytotoxicity and desmutagenic activity were investigated. From the cryophyllized S. JatiuscuJa, SL-l, SL-2 and SL-3 were purified by solvent extractions and HPLC.SL-2 was crystallized in benzene-diethyl ether solvent. On the EI-MS spectra, it was found that they had three bromines in their structure which showed typical signal strength ratios at $M^+, [M+2]^+, [M+4]^+, [M+6]^+ (13: 38: 37: 12)$. $SL-l$ was identified as 2,3,6-tribromo-4,5-dihydroxybenzyl alcohol ($C_8H_7Br_3O_3, MW=374$) by NMR and MS spectra. SL-2 was assigned as 2,3,6-tribromo-4,5-dihydroxybenzyl methyl ether ($C_8H_7Br_3O_3, MW=388$) and confirmed by X-ray crystallographic analysis. SL-3 was presumed as an isomer of SL-2. Methanol extract of the S. latiuscula showed antimicrobial activities against all strains tested (bacteria, 15 strains; yeasts, 17 strains; fungi, 4 strains), much or less. The strongest inhibition activity of the methanol extract was to the Vibrio mimicus ($50 {\mu}g/ml$) and V. vulnificus ($50 {\mu}g/ml$). The mice injected intraperitoneally with 3 mg of SL-l and 5 mg of 5L-2 showed no acute toxicity response. SL-2 showed higher desmutagenic activity than SL-l against PhIP and MeIQx.

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A Tumor Growth Inhibitory Substance Isolated from Panax ginseng (고려홍삼분말중의 항종양 활성물질)

  • Katano Mitsuo;Yamamoto Hiroshi;Matsunaga Hisashi
    • Proceedings of the Ginseng society Conference
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    • 1988.08a
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    • pp.33-35
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    • 1988
  • During a series of studies aimed at isolation of the tumor growth inhibitory substance from Panax ginseng. we found a new type of antitumor substance. The substance was isolated from a powder of the root of Panax ginseng C.A. Meyer. which is commonly used for various diseases as a commercial medical drug by the name of Korean Red Ginseng Powder in Japan. Data from infrared spectra proton and carbon-13 nuclear magnetic resonance. and high resolution mass spectra were identical with those of panaxytriol. Panaxytriol isolated from Korean Red Ginseng Powder (Nikkan Korai Ninjin Co.. Ltd.. Japan) inhibited the growth of several kinds of human and murine malignant cells in vitro. Although the detailed mechanism of cell growth inhibition by panaxytriol is yet to he elucidated. panaxytriol's action appeares to be more dose-dependent than time-dependent.

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Synthesis and Characterization of UO2(VI), Th(IV), ZrO(IV) and VO(IV) Complexes with Schiff-Base Octaazamacrocyclic Ligands (Schiff-염기인 옥타아자-거대고리 리간드의 UO2(VI), Th(IV), ZrO(IV) 및 VO(IV) 착물 합성 및 특성)

  • Mohapatra, Ranjan Kumar;Dash, Dhruba Charan
    • Journal of the Korean Chemical Society
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    • v.54 no.4
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    • pp.395-401
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    • 2010
  • A series of macrocyclic complexes of the type [M(L/L')$(NO_3)_n$].$mH_2O$ and [VO(L/L')($SO_4$)].$2H_2O$, where L/L' is a Schiff base "3,4,10,11-tetraphenyl/tetramethyl-1,2,5,6,8,9,12,13-octaaza cyclotetradeca-2,4,9,11-tetraene-7,14-dithione" derived from thiocarbohydrazide (TCH), benzilmonohydrazone (BMH)/diacetylmonohydrazone (DMH) and carbon disulphide, M = $UO_2$ (VI), Th(IV) and ZrO(IV), n = 2, 4, m = 2, 3, have been synthesized via metal ion template methods. The complexes are characterized on the basis of elemental analysis, thermal analysis, molar conductivity, magnetic moment, electronic, infrared and $^1H$-NMR spectral studies. The ESR and cyclic voltammetry studies of the vanadyl complexes have been carried out. The results indicate that the VO(IV) ion is penta-coordinated yielding paramagnetic complexes; $UO_2$(VI) and ZrO(IV) ions are hexacoordinated where as Th(IV) ion is octa-coordinated yielding diamagnetic complexes of above composition.

Synthesis of Renewable Resource-derived Furan-based Epoxy Compounds and Their Adhesive Property (재생자원 유래 퓨란계 에폭시 화합물의 합성 및 접착 특성)

  • Lee, Jae-Soung;Lee, Sang-Hyeup;Jeong, Jaewon;Kim, Baekjin;Cho, Jin Ku;Kim, Hyun Joong
    • Journal of Adhesion and Interface
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    • v.11 no.2
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    • pp.41-49
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    • 2010
  • Furan-containing epoxide monomers (8, 9) were designed and synthesized as carbon-neutral, environment-friendly adhesion material. Bicyclic skeleton were constructed using the Diels-Alder reaction of furan and methyl acrylate, both readily accessible starting material from a biomass via bio-refinery process. After reduction of ester functionality, resulting hydroxyl moieties were coupled to epichlorohydrin to provide the epoxy-functionalized furanic monomers (8, 9). The structure of new furanic monomers was confirmed by $^1H$ and $^{13}C$ NMR spectroscopy. As UV-curable monomers, basic properties such as UV curing time and the extent of UV curing were evaluated by photo DSC. Photo-curing shrinkages were measured by linear variable differential transformer transducer (LVDT) and the effect of molecular structure on shrinkage was considered. In addition, new synthetic compounds showed the shear strength over 3 MPa when they were photo-cured between polycarbonate plates, which indicates these compounds are feasible to use as photo-curable adhesive materials.

Molecular Structure of PCP Pincer Complexes: Poisoning Catalyst on the Dehydrogenation of Alkanes (알칸의 탈수소화반응에서의 촉매독 화합물의 분자구조)

  • Lee Ji Hyun;Chun Sang Jin;Kwon Ki Hyeok;Lee Do Weon
    • Korean Journal of Crystallography
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    • v.16 no.1
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    • pp.43-53
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    • 2005
  • The dihydrido P-C-P pincer complex, $IrH_2{C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (1), was successfully prepared from the reaction of the hydrochloride complex, $IrClH (C_6H_3-2,6-(CH_2PBu_2^t)_2}$, and super acid $(LiBEt_3H)$ under 1 atm of hydrogen in pentane solution at room temperature and followed by Heating at $130^{\circ}C$ in vacuo. Jensen recently found that the dihydrido P-C-P pincer complex 1 is a highly active homogeneous catalyst for the transfer dehydrogenation of alkanes with unusual longterm stability at temperatures as high as $200^{\circ}C$. The treatment of dihydrido complex 1 with nitrogen, water, carbon dioxide, and carbon monoxide in presence of tert-butylethylene (the) at room temperature in an appropriate solution gave the dinitrogen complex, $[Ir{C-6H_3-2,6-(CH_2PBu_2^t)_2}]_2({\mu}-N_2)$ (2), the hydrido hydroxyl complex, $IrH(OH){C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (3), the carbon dioxide complex, $Ir({\eta}^2-CO_2) {C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (including the bicarbonate complex, $IrH({\kappa}^2-O_2COH){C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(4))$, and the carbonyl complex, $Ir(CO) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(5)$ (including the carboxyl complex, $IrH(C(O)OH) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(6))$, in good yield, respectively. These P-C-P iridium complexes were isolated and characterized by $^1H,\;^{13}C,\;^{31}P\; NMR$, and IR spectroscopy. In addition, the complexes (1-6) were characterized by a single crystal X-ray crystallography. These complexes account for these small molecules' inhibition of dehydrogenation of alkanes catalyzed by the dihydrido complex 1.

Transdermal Drug Release of Polymer Matrix of Unsaturated Poly(3-hydroxyalkanoate) (불포화 폴리(3-히드록시알칸오에이트)를 기질로 한 경피제제의 약물방출)

  • 이수홍;신병철;이영하;김형우;김영백;김승수
    • Polymer(Korea)
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    • v.27 no.6
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    • pp.536-541
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    • 2003
  • Unsaturated poly(3-hydroxyalkanoate) (UPHA) was biosynthesized and the properties of drug delivery using the polymer matrix were investigated. The biosynthesis of UPHA was carried out by pH-stat fed batch fermentation of Pseudomonas oleovorans (ATCC 29347) grown solely with 10-undecenoic acid as a carbon source. The physical and chemical properties of the biosynethesized UPHA were characterized using NMR, FT-IR, GPC and DSC. The drug release experiments were carried out using HPLC with a diffusion cell fur the release amount of ketoprofen as model drug. The effects of crosslinking degree, patch thickness, and enhancer on the drug release were studied. The drug release rate was linearly decreased and consistent with increased crosslinking degree of the polymer matrix. The duration of drug release was enhanced by the Increased patch thickness. The drug release rate was increased with increased amount of propylene gylcol as an enhancer.