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

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Triterpenoid glycosides from rosa rugosa

  • Young, Han-Suk;Park, Jong-Cheol;Choi, Jae-Sue
    • Archives of Pharmacal Research
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    • v.10 no.4
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    • pp.219-222
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    • 1987
  • From the underground parts of Rosa rugosa(Rosaceae), 28-0-glucosides of euscaphic acid, tormentic acid and arjunic acid were isolated and characterized by spectral data.

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NMR Relaxation Study of Segmental Motions in Polymer-n-Alkanes

  • Chung Jeong Yong;Lee Jo Woong;Park Hyungsuk;Chang Taihyun
    • Bulletin of the Korean Chemical Society
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    • v.13 no.3
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    • pp.296-306
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    • 1992
  • $^{13}C$ spin-lattice relaxation times were measured for n-alkanes of moderate chain length, ranging from n-octane to n-dodecane, under the condition of proton broad-band decoupling within the temperature range of 248-318 K in order to gain some insight into basic features of segmental motions occurring in long chain ploymeric molecules. The NOE data showed that except for methyl carbon-13 dipole-dipole interactions between $^{13}C$ and directly bonded $^1H$ provide the major relaxation pathway, and we have analyzed the observed $T_1data$ on the basis of the internal rotational diffusion theory by Wallach and the conformational jump theory by London and Avitabile. The results show that the internal rotational diffusion constants about C-C bonds in the alkane backbone are all within the range of $10^9\;-10^10\;sec^{-1}$ in magnitude while the mean lifetimes for rotational isomers are all of the order of $10^{-11}\;-10^{-10}$ sec. Analysis by the L-A theory predicts that activation energies for conformational interconversion between gauche and trans form gradually increase as we move from the chain end toward the central C-C bond and they are within the range of 2-4 kcal/mol for all the compounds investigated.

Ginsenoside $Rg_5$, A Genuine Dammarane Glycoside from Korean Red Ginseng

  • Kim, Shin-Il;Park, Jeong-Hill;Ryu, Jae-Ha;Park, Jong-Dae;Lee, You-Hui;Park, Jae-Hyun;Kim, Tae-Hee;Kim, Jong-Moon;Baek, Nam-In
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.551-553
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    • 1996
  • A genuine dammarane glycoside, named ginsenoside $Rg_{5}$, has been isolated by repeated column chromatography and preparative HPLC from the MeOH extract of Korean red ginseng (Panax ginseng C.A. Meyer). The chemical structure of ginsenoside$ Rg_{5}$ was determined as $3-O-[{\beta}-D-glucopyranosyl (1{\rightarrow}2)-{\beta}-D-glucopyranosyl]$ dammar-20(22), $24-diene-3{\beta},12{\beta}-diol$ by spectral and chemical methods. The stereostructure of a double bond at C-20(22) of ginsenoside $Rg_{5}$ was characterized as (E) from the chemical shift of C-21 in the $^{13}C-NMR $and a NOESY experiment in the $^{1}H-NMR$.

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Backbone NMR Assignments of a Prokaryotic Molecular Chaperone, Hsp33 from Escherichia coli

  • Lee, Yoo-Sup;Won, Hyung-Sik
    • Journal of the Korean Magnetic Resonance Society
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    • v.16 no.2
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    • pp.172-184
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    • 2012
  • The prokaryotic molecular chaperone Hsp33 achieves its holdase activity upon response to oxidative stress particularly at elevated temperature. Despite many structural studies of Hsp33, which were conducted mainly by X-ray crystallography, the actual structures of the Hsp33 in solution remains controversial. Thus, we have initiated NMR study of the reduced, inactive Hsp33 monomer and backbone NMR assignments were obtained in the present study. Based on a series of triple resonance spectra measured on a triply isotope-[$^2H/^{13}C/^{15}N$]-labeled protein, sequence-specific assignments of the backbone amide signals observed in the 2D-[$^1H/^{15}N$]TROSY spectrum could be completed up to more than 96%. However, even considering the small portion of non-assigned resonances due to the lack of sequential connectivity, we confirmed that the total number of observed signals was quite smaller than that expected from the number of amino acid residues in Hsp33. Thus, it is postulated that peculiar dynamic properties would be involved in the solution structure of the inactive Hsp33 monomer. We expect that the present assignment data would eventually provide the most fundamental and important data for the progressing studies on the 3-dimensional structure and molecular dynamics of Hsp33, which are critical for understanding its activation process.

Metal-Dinitrosyl Complexes(Ⅳ) : Synthesis and Characterization of Symmetric and Asymmetric Dinuclear Molybdenum and Tungsten Complexes (금속-디니트로실 착물 (제 4 보) : 몰리브덴과 텅스텐의 대칭 및 비대칭 이핵 착물의 합성과 특성)

  • O, Sang O;Mo, Seong Jong
    • Journal of the Korean Chemical Society
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    • v.38 no.7
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    • pp.485-495
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    • 1994
  • Several new symmetric and asymmetric homo and hetero dinuclear complexes of the type $[Cl(dppp)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$ and $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$(M,M'= Mo or W; phen = 1,10-phenanthroline; dppp = 1,3-bis(diphenylphosphino)propane; pyz = 1,4-pyrazine) were synthesized in three-steps starting from $[M(NO)_2Cl_2]_n(M = Mo, W)$. The final products were purified by eluting it through silica gel column ($2{\times}20$ cm) with acetone as the eluent. Characterization of these complexes and some related complexes was accomplished through UV-vis., $^1H$-NMR, $^{13}C$-NMR and IR spectroscopies as well as elemental analysis. The infrared spectra indicate that the NO groups occupy cis-positions of the octahedral. The $^1H$ and $^{13}C-NMR$ data for the new compounds revealed a dimeric structures with bridged pyz.

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Synthesis and Properties of Conjugated Cyclopolymers Bearing Fluorene Derivatives

  • Gal Yeong-Soon;Jin Sung-Ho;Lee Hyo-San;Kim Sang Youl
    • Macromolecular Research
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    • v.13 no.6
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    • pp.491-498
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    • 2005
  • Fluorene-containing, spiro-type, conjugated polymers were synthesized via the cyclopolymerization of dipropargylfluorenes (2-substituted, X=H, Br, Ac, $ NO_{2}$) with various transition metal catalysts. The polymerization of dipropargylfluorenes proceeded well using Mo-based catalysts to give a high polymer yield. The catalytic activities of the Mo-based catalysts were found to be more effective than those of W-based catalysts. The palladium (II) chloride also increased the polymer yield of the polymerization. The polymer structure of poly(dipropargylfluorene)s was characterized by such instrumental methods as NMR ($^{1}H_{-}$, $^{13}C_{-}$), IR, UV-visible spectroscopies, and elemental analysis as having the conjugated polymer backbone bearing fluorene moieties. The $^{13}C_{-}$NMR spectral data on the quaternary carbon atoms in polymers indicated that the conjugated cyclopolymers have the six-membered rings majorly. The poly(dipropargylfluorene) derivatives were completely soluble in halogenated and aromatic hydrocarbons such as methylene chloride, chloroform, benzene, toluene, and chlorobenzene. The poly(dipropargylfluorene) derivatives were thermally more stable than poly(dipropargylfluorene) itself, and X-ray diffraction analyses revealed that the polymers are mostly amorphous. The photoluminescence peaks of the polymers were observed at about 457-491 nm, depending on the substituents of fluorene moieties.

Structure Identification of 1,2-Disubstituted Chiral Calix[4]arene : X-Ray and NMR Analysis of 25-(3,5-Dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene

  • 박영자;신정미;남계춘;김종민;국승근
    • Bulletin of the Korean Chemical Society
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    • v.17 no.7
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    • pp.643-647
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    • 1996
  • 1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

Tautomerism and Alkylation of 5-Amino-2H-1,2,4-thiadiazoline-3-one (5-Amino-2H-1,2,4-thiadiazoline-3-one의 토토머화 현상과 알킬화 반응)

  • Cho, Nam Sook;Park, Young Cheol;Ra, Do Young;Kang, Sungkwon
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.564-571
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    • 1995
  • 5-Amino-2H-1,2,4-thiadiazoline-3-one has been prepared from 2-thiobiuret through a oxidative cyclization under basic hydrogen peroxide condition. Lactam-lactim tautomerism of 5-amino-2H-1,2,4-thiadiazoline-3-one has been examined by spectroscopic methods and ab initio molecular orbital calculation. These results were shown that 5-amino-2H-1,2,4-thiadiazoline-3-one exists as lactam form. Reaction conditions for alkylating 5-amino-2H-1,2,4-thiadiazoline-3-one with alkyl halides in the presence of various bases were studied in DMF and $H_2O$-THF two phase system. $Li_2CO_3$ base in DMF method gave best result in this investigation. The alkylation has been taken place at N-2 position. The identification of the product is confirmed by spectral data of IR, $^1H$ NMR and $^13C$ NMR and the comparison of authentic sample, 5-amino-2-methyl-1,2,4-thiadiazolidine-3-one, obtained from the oxidative cyclization of 5-methyl-2-thiobiuret.

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