• 제목/요약/키워드: 2 D-NMR

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An NMR Study of Unequal Site Exchange of 9-Methyl Group in Triptycene by Spin-Lattice Relaxation and 2D-EXSY Experiments

  • Cho, Jang-Geun;Ahn, Sang-Doo
    • 한국자기공명학회논문지
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    • 제11권1호
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    • pp.1-9
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    • 2007
  • An unequal site exchanging system induced by restricted rotation of 9-methyl group in 1,8-dichloro-9-triptycene has been studied by spin-lattice relaxation and 2D-EXSY experiments. The exchange rate obtained from relaxation studies is very well coincident to the result of line shape analysis, and the difference of the relaxation times ($T_1$) in two different sites has an important role to analyze 2D-EXSY experimental data.

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Complete assignments of $^{1}H$ and $^{13}C NMR$ spectra of Chivosazole F

  • Park, Jung-Rae;Jongheonn Shin;Kim, Jin-Cheol;Ahn, Jong-Woong
    • 한국자기공명학회논문지
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    • 제5권2호
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    • pp.91-98
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    • 2001
  • The $^1$H and $^{13}$ C NMR spectra of chivosazole F from Sorangium cellulosum were completely assigned by a combination of ID and 2D NMR techniques. The configurations of double bonds were confirmed from the ROESY spectra. The stereochemistry at asymmetric carboncenters was partially assigned on the basis of the results of NOE analysis.

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Trichoderma koningii에서 분비되는 .$\beta$-D-glucosidase의 반응산물에 대한 핵자기공명분석 ($^{1}$H-NMR spectroscopic evidence on the glycosidic linkages of the transglycosylated products of low-molecular-weight $\beta$-D-glucosidase from trichoderma koningii)

  • 이헌주;정춘수;강사욱;하영칠
    • 미생물학회지
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    • 제27권1호
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    • pp.35-42
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    • 1989
  • The mode of transglycosylation reaction observed during the action of low-molecular-weigh $\beta$-D-glucosidase ($\beta$-D-glucoside glucohydrolase, EC3.2.1.21) purified from Trichoderma koningii ATCC 26113 was investigated using $^{1}H$-NMR spectroscopy. The enzyme was purified by the series of procedures including ammonium sulfate precipitation, and fractionations by column chromatographies on Bio-Gel P-150, DEAE-Sephadex A-50, and SP-Sephadex C-50. The final purification was performed by the band eluation after preparative polyacrylamide gel electrophoresis. The enzyme showed its molecular size of 78,000 through the analysis of sodium dodecyl sulfate-polyacrylamide gel electrophoresis and its isoelectric point of 5.80 through the analysis of analytical isoelectric focusing. The H-1 proton resonances were analyzed. After the reaction of the enzyme with cellobiose, the reaction products were separated by high performance liquid chromatography using refractive index detector. H-1 resonances of the products were consisted with those of gentiobiose [$\beta$-D-glucopyranosyl--(1,6)-D-glucopyranose], and cellotriose [$\beta$-D glucopyranosyl-(1,4)-$\beta$-D-glucopyranosyl]-(1,4)-D-glucopyranose] with minor resonances of sophorose [$\beta$-D-glucopyranosyl-(1,2)-D-glucopyranose], respectively.

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솜양지꽃 뿌리로부터 스테로이드와 트리테르페노이드 성분의 분리 (Isolation of Two Steroids and a Triterpenoid from the Roots of Potentilla discolor)

  • 박희준;이경태;박종희
    • 생약학회지
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    • 제38권4호
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    • pp.354-357
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    • 2007
  • Three compounds (1-3) were isolated from the roots of Potentilla discolor (Rosaceae). The structure of compounds 1-3 were elucidated as stigmast-5-en-3-ol $({\beta}-sitosterol,\;1),\;2,19{\alpha}-dihydroxy$-2-oxo-urs-1,12-dien-28-oic acid (fupenjic acid, 2), 3-O-${\beta}$-D-glucopyranosylstigmast-5-en-3-ol (${\beta}-sitosterol\;{\beta}-D-glucopyranoside, 3) based on physical and spectroscopic data. $^{13}C-NMR$ assignments were completed by 2D-NMR technique. The three compounds were firstly isolated from Potentilla discolor.

Separation and Identification of Cyclic Oligomers in Poly (trimethylene terephthalate)

  • Min Bum-Chan;Lim Byung-Ho;Ko Suk-Yen
    • 한국자기공명학회논문지
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    • 제10권1호
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    • pp.38-45
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    • 2006
  • The NMR and MS techniques were applied to identification and quantitative analysis of oligomers in a commercialized poly (trimethylene terephthalate). Oligomers in a commercialized poly (trimethylene terephthalate) were extracted via a dissolving and reprecipitation method. Analysis of the components of the extract using NMR and MS revealed that it contained mainly cyclic oligomers with degrees of polymerization of 2, 4 and 5 (dimer, tetramer and pentamer). Trimer and cyclic oligomers with degrees of polymerization of more than 6 were not found in the extract in the present study. Quantitative analysis of dimer was performed by NMR spectroscopy.

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Complete Assignments of the 1H and 13C NMR Data of Flavone Derivatives

  • Moon, Byoung-Ho;Lee, Young-Shim;Shin, Choon-Shik;Lim, Yoong-Ho
    • Bulletin of the Korean Chemical Society
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    • 제26권4호
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    • pp.603-608
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    • 2005
  • The $^1H\;and\;^{13}C$ chemical shifts of flavone and its five derivatives were determined completely using the basic 1D and 2D NMR experiments and molecular modeling. Of the six compounds used for our experiments, the NMR data of three compounds were published previously, but we found that the data of two compounds included wrong assignments. Therefore, we report the corrected data and the complete assignments of NMR data of the other three compounds.

Structure Elucidation for New Sestertepene Alkaloids from the Sponge Sacotragus sp.

  • Rho, Jung-Rae;Shin, Jong-Heon;Lee, Hyi-Seung
    • 한국자기공명학회논문지
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    • 제7권1호
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    • pp.55-61
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    • 2003
  • Sarcotragins C(1) and D(2), two novel compounds, have been isolated from the sponge Sarcotragus sp. collected from Jaeju Island, Korea. The structures of these compounds have been determined to be linear sesterterpene alkaloids on the basis of combined 1D and 2D NMR experiments. The stereochemistry involved was established by comparison of the NMR data with those reported for a similar compound.

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Isolation and structure elucidation of a catechin glycoside with phospholipase $A_2$ inhibiting activity from Ulmi cortex

  • Park, Sunghyouk;Goo, Yang-Mo
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 1995년도 춘계학술대회
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    • pp.58-58
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    • 1995
  • 식물에서부터 새로운 소염작용제를 개발하기 위하여 여러식물을 대상으로 염증반응의 초기단계에서 중요한 역할을 하는 것으로 알려진 Phospholipase $A_2$에 저해활성을 갖는 물질을 검색하였고 그 중 강한 억제활성을 보인 유근피에서 유효성분을 분리하였다. 유근피의 에칠 아세테이트 분획에 대하여 실리카겔 크로마토그래피, Sephadex LH-20 크로마토그래피, 분취 박막 크로마토그래피를 수행하여 phenol성 -OH기를 갖는 활성성분인 PSH-II-84-1를 분리하였다. $^1$H-NMR 신호의 양상과 짝지움 상수 값에서 분리된 물질은 (+)-catechin 의 당 유도체로 확인되었다. $^{13}$C-NMR 자료를 분석하여 치환된 당은 D-apiofuranose로 확인되었다. 방향족환의 $^{l3}$C-NMR 신호들은 extended Huekel theory를 응용하여 얻은 net charge 계산 값과 상관시켜 할당하였다. 이상의 구조연구 결과 이 물질은 (+)-catechin-7-0-$\beta$-D-apiofuranoside로 밝혀졌다. (+)-catechin-7-0-$\beta$-D-apiofuranoside의 효소억제활성은 Type II Phospholipase $A_2$에 대하여 $IC_{50}$/이 600$\mu$M이었다.다.

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A Conformational Study of Linkage Positions in Oligosaccharides Investigated by 2-D NMR Spectroscopy and Molecular Modeling

  • Yoo Yoon, Eun-Sun
    • Bulletin of the Korean Chemical Society
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    • 제24권3호
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    • pp.339-344
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    • 2003
  • The conformation of synthetic oligosaccharide can be elucidated by employing molecular modeling and highfield proton NMR (nuclear magnetic resonance) spectroscopy. Information with respect to the composition and configuration of saccharide residues and the sequence and linkage positions of the oligosaccharide can be obtained by employing a variety of one- and two-dimensional NMR techniques and molecular modeling. These techniques are also useful in establishing the solution conformation of the oligosaccharide moiety. This study is focused on the elucidation of linkage positions of synthetic trisaccharides, Gal(β1-4)Glc(β1-3)Glc, Gal(β1-4)Glc(β1-4)Glc and Gal(β1-4)Glc(β1-6)Glc.

계면활성제 수용액에서 미셀형성(제3보) -비이온성과 이온성계면활성제의 혼합 미셀에 있어 자기확산 및 프로톤 이완- (Micelle Formation of Surfactant Solution(3) -Self-Diffusion and 1H Relaxation for Mixed Micelle of Nonionic and Ionic Surfactants-)

  • 최성옥;곽광수;박흥조;남기대
    • 공업화학
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    • 제10권6호
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    • pp.876-880
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    • 1999
  • 이온성과 비이온성계면활성제의 혼합 미셀 용액의 자기확산계수는 NMR FT-PGSE법으로 측정하였다. 또한 프로톤 NMR 피크의 폭을 관찰하였다. 연구된 계는 $C_{12}EO_5/SDS/D_2O$, $C_{12}EO_5/DTAC/D_2O$$C_{12}EO_8/SDS/D_2O$의 혼합계이다. 모든 시료에서 솔벤트와 계면활성제의 몰비는 일정하고 계면활성제의 혼합비는 다양하게 실험을 하였다. $C_{12}EO_5$ 계에서 계면활성제의 자기확산계수는 이온성계면활성제의 혼합비가 약 25%일 때 최소치를 나타내었다. 비이온성계면활성제가 이온성계면활성제로 치환됨에 따라서 자기확산계수가 감소하는 것은 미셀간의 반발력이 증가하기 때문이다. 이온성계면활성제의 높은 분율에서 자기확산계수가 증가하는 것은 미셀의 크기가 감소하기 때문이다. $C_{12}EO_8$ 계에서 계면활성제의 혼합비의 효과는 분자의 기하학적 구조와 큰 관능기의 면적 때문에 거의 없다. 프로톤 NMR 피크와 자기확산계수는 상호 밀접한 관계를 나타내고 알킬 사슬의 메틸렌 시그날의 넓혀짐 현상은 자기확산계수가 작을 때 나타난다.

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