• Title/Summary/Keyword: 2D NMR techniques

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Spectral and Thermal Properties of Some Uranyl Complexes of Some Schiff-Bases Derived from Glycylglycine

  • Sh. A. Sallam;M. I. Ayad
    • Journal of the Korean Chemical Society
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    • v.47 no.3
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    • pp.199-205
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    • 2003
  • Complexes of uranyl ion $UO^{+2}_2$with Schiff-bases obtained by condensing glycylglycine with salicylaldehyde; 2-hydroxy-1-naphthaldehyde, 2,3-dihydroxybenzaldehyde, and 2,4-dihydroxybenzaldehyde have been synthesized and characterized through elemental analysis, conductivity measurements, magnetic susceptibility determinations, u.v., i.r. and $^1H$ nmr spectra as well as d.t.a., t.g. and d.s.c. techniques. Structures and mechanisms of thermal decomposition are proposed.

Solution State Structure of pB1, the Mimotopic Peptide of Apolipoprotein B-100, by NMR

  • Lee, Sung-Ran;Kim, Dae-Sung;Kim, Hyo-Joon;Lee, Yong-Woo;Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.25 no.12
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    • pp.1845-1849
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    • 2004
  • Apolipoprotein B-100 (Apo-B100) is a major protein component for low density lipoproteins (LDL). A number of mimetic peptides of Apo-B100 were screened from the phase-displayed random peptide library by utilizing monoclonal antibody (B9). Mimetic peptide for B9 epitope against apo B-100 was CRNVPPIFNDVYWIAF (pB1). From the BLAST search, the mimetic peptide pB1 had 40% homology with apo B-100. As a result of the structural determination of this mimotope using homo/hetero nuclear 2D-NMR techniques and NMR-based distance geometry (DG)/molecular dynamic (MD) computations, DG structure had low penalty value of 0.3-0.6 ${\AA}^2$ and the total RMSD was 0.5-1.5 ${\AA}. Moreover, pB1 structure included a weak $3_{10}$-helix from $Ile^7$,/TEX> to $Trp^{13}$.

Thymol Derivatives form Carpesium divaricatum

  • Zee, Ok-Pyo;Kim, Dae-Keun;Lee, Kang-Ro
    • Archives of Pharmacal Research
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    • v.21 no.5
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    • pp.618-620
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    • 1998
  • Four thymol derivatives, 2,5-dimethoxythymol (1), 2-methoxythymol isobutyrate (2), 10-isobutyloxy-8,9-epoxythymolisobutyrate (3) and 10-(2-methylbutyloxy)-8,9-eposythymolisobutyrate (4) were isolated from the aerial parts of Carpesium divaricatum. the structures were elucidated by high field 1D and 2D NMR techniques.

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A New Epoxynaphthoquinol from Rumex japonicus

  • Zee, Ok-Pyo;Kim, Dae-Keun;Kwon, Hak-Cheol;Lee, Kang-Ro
    • Archives of Pharmacal Research
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    • v.21 no.4
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    • pp.485-486
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    • 1998
  • A new epoxynaphthoquinol derivative, 3-acetyl-2-methyl-1, 5-dihydroxy-2,3-epoxynaphthoquinol (I), was isolated from the root of Rumex japonicus. The structure was elucidated by high field 1D and 2D NMR techniques.

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Steroidal Saponins from the Rhizomes of Asparagus oligoclonos and their Antibacterial Activity (방울비짜루(Asparagus oligoclonos)로부터 분리한 스테로이드 사포닌의 항균활성)

  • Seong, Jae-Duck;Park, Seung-Yong;Oh, Sei-Ryang;Kwack, Yong-Ho;Kim, Geum-Soog
    • Applied Biological Chemistry
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    • v.43 no.2
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    • pp.136-140
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    • 2000
  • Two steroidal saponins were isolated from MeOH extract of the rhizomes of Asparagus oligoclonos. Using the spectroscopic techniques of $^1H,\;^{13}C$ NMR and 2D NMR, they were identified as $3-O-[{\beta}-D-glucopyranosyl-(1{\rightarrow}2)-{\beta}-D-glucopyranosyl]-(25S)-spirostan-3{\beta}-ol$ and $3-O-{{\beta}-D-glucopyranosyl-(1{\rightarrow}2)-[{\beta}-D-xylopyranosyl-(1{\rightarrow}4)]-{\beta}-D-glucopyranosyl}-(25S)-spirostan-3{\beta}-ol$, respectively. They were first isolated from A. oligoclonos. The in vitro antibacterial activities as well as antibacterial spectrums against 20 bacteria strains were investigated with MIC test. Both saponins inhibited the growth of 10 bacteria strains at the concentration of$100\;{\mu}g/ml$.

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Structural Studies of Copper(II)-Hippuryl-L-histidyl-L-leucine(HHL) Complex by NMR Methods

  • Lee Seong-Ran;Jun Ji-Hyun;Won Ho-Shik
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.1
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    • pp.115-125
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    • 2006
  • Hippuryl-L-histidyl-L-leucine(HHL) is widely used as a substrate of angiotensin converting enzyme(ACE) cleaving the neurotransmitter angiotensin(I) to the octapeptide angiotensin(II). The structure of the substrate molecules should provide information regarding the geometric requirements of the ACE active site. For the purpose of determination of in vivo reaction, metallo(Cu, Zn)-HHL complexes were synthesized and the degree of complex formation were identified by MALDITOF, ESI mass spectrometric analysis. Tn addition, the pH-dependent species distribution curves were obtained by potentiometric titration. Nitrogen atoms of imidazole ring and oxygen atom of caboxylate groups in the peptide chain were observed to be participated in the metal complex formation. After purification of complexes further structural characterization were made by utilizing UV-Vis, electrochemical methods and NMR. Complete NMR signal assignments were carried out by using 2D-spectrum techniques COSY, TOCSY, NOESY, HETCOR. A complex that two imidazole and carboxylate groups are asymmetrically participating to coordination mode was predicted to the solution-state structure of $Cu(II)-HHL_2$ based on $^{13}C-NMR$ signal assignment and NOE information.

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A New Apotirucallane-type Triterpenoid from the Fruit of Melia azedarach

  • Jin, Qinghao;Lee, Chul;Lee, Jin Woo;Lee, Moon-Soon;Lee, Mi Kyeong;Hwang, Bang Yeon
    • Natural Product Sciences
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    • v.19 no.4
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    • pp.342-346
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    • 2013
  • A new apotirucallane-type triterpenoid, $3{\alpha}$-tigloylsapelin D (1) together with five known triterpenoids such as meliasenin B (2), sendanolactone (3), (-)-$12{\beta}$-hydroxykulactone (4), cinamodiol (5), and $3{\alpha}$-hydroxytirucalla-7,24(25)-dien-6-oxo-21,16-olide (6) were isolated from the fruits of Melia azedarach. Their structures were established on the basis of various NMR spectroscopic analyses including 2D-NMR techniques (HSQC, HMBC, and NOESY) and HR-FAB-MS data.

Solid-state NMR Studies of Miscibility and Morphology in Blends of Bisphenol-A type Polycarbonate and Poly (ester-ether) Elastomer

  • Kim, Yongae
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.1
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    • pp.19-28
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    • 2001
  • Miscibility and morphology in blends of bisphenol-A type polycarbonate and poly (ester-ether) elastomer with different compositions are studied by solid-state NMR spectroscopy. $^{13}$ C Solid-state NMR of CP/MAS/TOSS/DD, CP/MAS/DD, inversion recovery CP/MAS/DD, and 2D rotor driven spin diffusion techniques are used to identify the miscibility, morphology, and transesterification in blends. The blends of PC /BT elastomer with 15% to 42% of soft segment seem to be single phase miscible mixing and those of PC/PBT and PC/PBT elastomer with 62% of soft segment are cocontinuous two phase immiscible mixing. No significant transesterification reactions are observed in blends with different compositions.

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Biopharmaceutical Studies on the Alkanol Esters of Naproxen(I) -Studies of 3 Kinds Alkanol Esters of Naproxen- (나프록센의 Alkanol 에스테르류에 관한 생물약제학적 연구 I -3종의 Alkanol 에스테르의 합성-)

  • 백우현;김종갑
    • YAKHAK HOEJI
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    • v.30 no.3
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    • pp.121-127
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    • 1986
  • Three new alkanol esters of d-2-(6-methoxy-2-naphthyl)propionic acid, NAPROXEN were synthesized by esterification of sodium naproxen with chloralcohols, such as 2-chloroethanol, 3-chloro-1, 2-propanediol and $\beta$-chloroethoxyethanol in dimethylformamide. These new esters were obtained with comparably high yield and identified by elemental analysis, UV, IR and NMR techniques.

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The Structure of Kushenol M from Sophora flavescens

  • Ryu, Shi-Yong;Lee, Seung-Ho;No, Zaesung;Kim, Kye-Young;Lee, Sueg-Geun;Ahn, Jong-Woong
    • Archives of Pharmacal Research
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    • v.18 no.1
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    • pp.41-43
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    • 1995
  • The linkage pattem of two side chains i.e., a isopentenyl and a lavandulyl group in kushenol M(I), a flavonoid from Sophora flavescens was established by the aid of 2-D NMR techniques, especially DEPT, ${13}C-^1H$ COSY and COLOC experiments. Thus, I was unequivocally determined as (2R, 3R)-5, 7, 2', 4'-tetrahydroxy-6-isopentenyl-8-lavandulyflavanonol.

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