• 제목/요약/키워드: Carbon 13 NMR

검색결과 132건 처리시간 0.027초

NMR Spectroscopic Study of Quinolone Carboxylic Acid Derivatives

  • Dongsoo Koh;Lee, Inwon;Park, Jongmin;Lee, Hyeseung;Yoongho Lim
    • 한국자기공명학회논문지
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    • 제3권1호
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    • pp.52-59
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    • 1999
  • Authors synthesized common intermediates which are applicable for potential antibiotics. Their complete 13C and 1H NMR chemical shift data as well as carbon-and proton-fluorine coupling constants are reported. The knowledge of proton and carbon-fluorine coupling constants may help one assign the NMR data of the fluorinated quinolone derivatives. These results agree with the data published previously.

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리간드 N-Benzylisonitrosoacetylacetone Imine의 구조 (The Structure of Ligand, N-benzylisonitrosoacetylacetone Imine)

  • 이병교;오대섭;이흥락
    • 대한화학회지
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    • 제32권6호
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    • pp.549-556
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    • 1988
  • 이미 합성된 N-benzylisonitrosoacetylacetone $imine^1$의 유기용매내에서의 구조변화를 측정하기 위하여 여러가지 유기용매에서의 핵자기공명스펙트럼 및 Carbon-13 핵자기공명 DEPT 스펙트럼 등의 분광학적인 자료를 이용하였다. 그 결과 이 시약은 monoxime의 일종으로 용매 중에서 syn- 형과 anti- 형의 기하이성질체가 공존하고 있으며 각각이 토우토메리 현상을 일으키고 있다.

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13C-NMR에 의(依)한 알카리 모델리그닌의 착색구조(着色構造)에 관(關)한 연구(硏究) (Identification of the chromophoric structure in alkali model lignin by 13C-NMR)

  • 윤병호
    • 한국산림과학회지
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    • 제43권1호
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    • pp.14-19
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    • 1979
  • 펄프화중(化中)의 리그닌의 착색구조(着色構造)를 구명(究明)하기 위(爲)하여 바니릴알콜을 1규정농도(規定濃度)의 가성(苛性)소다로 90~180분간(分間) 질소하(窒素下)에 처리(處理)한 후(後) 공기중(空氣中)에 8시간(時間) 산화(酸化)하여 크로마토그라피로 착색물질(着色物質)을 분리(分離)했다. 이 물질(物質)은 $^{13}C$-NMR스펙트로로는 착색구조(着色構造)에 기인(基因)하는 케미칼쉬풀트는 보이지 않았다. 한편, 탄소(炭素)를 $^{13}C$으로 라벨한 바니릴알콜-[카비놀-$^{13}C$]을 상기(上記)와 같은 처리(處理)로 생성(生成)된 착색물질(着色物質)은 퀴논메티드로 귀속(歸屬)시킬 수 있는 101.7과 104.6 ppm에 케미칼쉬풀카 나타나므로 ${\alpha}$탄소(炭素)에 관여(關與)하는 착색구조(着色構造)임을 확인(確認)했다.

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Poly(styrene carbonate)의 합성 및 열분해에 의한 styrene carbonate의 제조 (Synthesis of Poly(styrene carbonate) and Preparation of Styrene Carbonate by Thermal Degradation)

  • 이윤배;신은정;유진이
    • 공업화학
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    • 제19권1호
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    • pp.133-136
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    • 2008
  • 온실 가스 가운데 하나인 이산화탄소를 줄이기 위한 연구의 일환으로 이산화탄소와 산화 스틸렌을 원료로 하고 zinc glutarate를 촉매로 하여 poly(styrene carbonate)를 합성하였다. 여러 가지 분광학적인(FT-IR, $^1H$-NMR, $^{13}C$-NMR, GC-MS) 분석결과 교대 공중합체임이 확인되었으며, MALDI법에 의하여 분자량($\bar{M}_n$)은 $5.0{\times}10^4$이며, 유리전이온도는 $88^{\circ}C$이고, 융융점은 $240^{\circ}C$로 밝혀졌다. 이 고분자를 열분해하면 고리형 카보네이트인 styrene carbonate가 생성되는 것도 확인하였다.

초임계 이산화탄소를 이용한 maca [Lepidium meyenii]의 지질 추출물로부터 macamides 분리 및 동정 (Isolation and Identification of Macamides from the Lipidic Extract of Maca [Lepidium meyenii] using Supercritical Carbon Dioxide)

  • 이승호;강정일;이상윤;하효철;송영근;변상요
    • KSBB Journal
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    • 제23권2호
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    • pp.153-157
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    • 2008
  • 생리활성이 뛰어난 마카의 지질 분획으로부터 macamides를 분리 동정하기 위해 본 연구에서는 초임계 이산화탄소 추출을 통해 마카 지질 추출물을 제조하여 재순환 분취용 HPLC로부터 2종의 macamides 물질을 분리 정제하였다. 분리된 2종의 macamides 물질의 구조 해석을 위해 LC/MS와 $^1H$-NMR과 $^{13}C$-NMR 분석을 실시한 결과 분자량이 384인 N-benzyl-5-oxo-6E,8E-octadecadienamide와 분자량이 346인 N-benzylhexadecanamide로 동정되었다. 본 연구를 통해 분리된 2종의 macamides는 향후 마카분말 및 마카제품의 macamides의 지표물질로 활용이 가능할 것으로 사료된다.

소목 추출물의 구조분석 (A Study on the Component Analysis of Sappan Wood Extracts)

  • 이상락;김인회;남성우
    • 한국염색가공학회지
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    • 제14권4호
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    • pp.229-239
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    • 2002
  • Colorants were extracted from the heartwood of sappan lin. with MeOH under reflux, and the concentrate or the powder of dye was prepared by low pressure concentration method using suitable organic solvent. Various components were isolated from sappan wood, and the chemical structure and mechanism of compound having the excellent antibacterial and deodorization properties were analyzed. The results obtained are as follows ; The seventeen components of sappan wood were seperated by HPLC chromatography, and the five components among them were existed more than 6% and the other components were existed lower than 0.6%. The resolving powers of the non-polar solvent and polar solvent systems were evaluated by their ability to resolve the samples. It showed that chloroform-methanol-water(800:150:10) system has the best resolving power. Although the seperation rate is very slow, polyamide C-100 column chromatography gives a clear seperation of sappan wood. On the basis of the spectrometric data such as IR, UV, $GC-Mass,\;^1H-NMR,\;^{13}C-NMR\;and\;^1H-^{ 13}C-NMR$, the chemical structure of compound haying the excellent antibacterial and deodorization properties was established as brazilin containing the functional groups such as two quaternary carbon, one benzyl carbon, methylene contiguous to oxygen and methylene caused by oxygen atom.

Intramolecualr cyclization of a dipyrromethane by an electrophilic aromatic substitution reaction producing a new chiral compound

  • Kim, Seung Hyun;Kim, Sung Kuk
    • 한국자기공명학회논문지
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    • 제22권4호
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    • pp.115-118
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    • 2018
  • Dipyrromethane 2 functionalized with 3-chloropropyl group on the meso carbon undergoes an unusual intramolecular electrophilic aromatic substitution reaction in the presence of $NaN_3$ instead of a simple nucleophilic substitution reaction. As a result, a new chiral dipyrromethane 1 was synthesized. In this reaction, the ${\beta}$-carbon of the pyrrole ring functions as a nucleophile while the carbon next to the chlorine atom acts as an electrophile. Interestingly, this reaction progresses even in the absence of an acid catalyst. Compound 1 was fully characterized by $^1H-^1H$ and $^1H-^{13}C$ COSY NMR spectroscopic analyses and the high resolution EI mass spectrometry.

항 단실 항체의 카르보닐탄소 유래 시그날의 귀속 (Assignment of the Carbonyl Carbon Resonances in Anti-Dansyl Antibodies)

  • 김하형;이광표
    • 약학회지
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    • 제39권5호
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    • pp.516-520
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    • 1995
  • The anti-dansyl antibodies were specifically labeled with stable isotope by growing hybridoma cells in serum-free medium. Assignments of the observed carbonyl carbon resonances have been determined by using $^{13}C-{15}N$ double labeling method in order to assign the Leu resonances. However, when the identical dipeptide appears more than twice in the polypeptide sequences, we applied the proteolytic fragments in the fragment-specific method. Carboxypep-tidase B-treated antibody has also been used to assign the Lys-447 in C terminal amino acid. These unambiguously assigned carbonyl carbon resonances in antibodies are thought to be useful in elucidating not only the structure of antibodies but also the structure-function relationship in the antibody by $^{13}C$ neuclear magnetic resonance spectroscopy.

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Carbon-13 CP MAS NMR Study on Structures of Octadecyl Chains Influenced by Co-Presence of 3-Aminopropyl Chains on SBA-15

  • Han, Oc-Hee;Bae, Yoon-Kyung;Jeong, Soon-Yong
    • Bulletin of the Korean Chemical Society
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    • 제29권2호
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    • pp.405-407
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    • 2008
  • Functionalized SAB-15 samples by octadecyltrimethoxysilane (OTC) were studied by 13C magic angle spinning (MAS) cross polarization (CP) nuclear magnetic resonance (NMR) spectroscopy. In the SBA-15 sample fully functionalized by 3-aminopropyltrimethoxysilane (APS) and OTC in 1:1 molar ratio, octadecyl chains were observed to have, on average, more trans conformation than those in the SBA-15 samples fully modified by OTC only. Our results confirm that long chain molecules tend to organize themselves better in the co-presence of short chain molecules on the surface of mesoporous materials by packing of the different length chains in an interdigitized fashion even when the short chains are long enough to have three carbons and a functional group at the ends. In addition, our results indicate that solid-state 13C CP MAS NMR spectroscopy is a simple and non-destructive method to probe the molecular structures of the domains composed of long alkyl chains.

NMR에 의한 anti-Ex-A IgG의 항원결합부위 해석 (Paratope Mapping of Anti-Ex-A IgG as Studied by NMR)

  • 김하형;이광표;가토 코이치;아라타 요우지
    • 약학회지
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    • 제40권4호
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    • pp.422-427
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    • 1996
  • The anti-Ex-A IgG was specifically labeled with stable isotopes, DL-His-2,4-$d_2$, L-Phe-$d_5$, L-Trp-$d_5$, L-Tyr-2,6-$d_2$ and L-[1-$^{13}C$]Trp, by growing hybridoma cell in serum-free medium. By use of NMR spectroscopy with selectively labeled Fab fragment, we applied a paratope mapping on antigen-antibody complex. Assignments of the observed carbonyl carbon resonances have been determined by using $^{13}C$-$^{15}N$ double labeling method in order to assign the Trp resonances. Photo CIDNP was also applied to investigate the antigen-binding site(s) on the surface residues of antibody. We found that Trp 36, which is located at the $V_H$ domain, is an important residue to bind to Ex-A, however, two Tyr on the surface of anti-Ex-A IgG plays no crucial role to bind to antigen. On the basis of these results, we demonstrate that stable isotope-aided NMR strategy can be extended to molecular structural analyses of the complex of an Fab fragment and a protein antigen.

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