• 제목/요약/키워드: NMR spectroscopic analysis

검색결과 205건 처리시간 0.026초

Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • 제25권11호
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

폴리이미드 LB 필름을 이용한 패터닝 및 생물전자 소자로의 응용에 관한 연구 (Studies on the Patterning of Polyimide LB Film and Its Application for Bioelectronic Device)

  • 오세용;박준규;정찬문;최정우
    • 폴리머
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    • 제26권5호
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    • pp.634-643
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    • 2002
  • 고분자 주사슬에 벤젠과 sulfonyloxvimide moiety를 가지고 있는 polyamic acid 초박막을 LB 기법을 이용하여 제조한 다음 200 $^{\circ}C$에서 1시간 동안 열처리에 의해 감광성 폴리이미드 LB 필름을 얻었다. Polyamic acid는 THF-pyridine 공용매를 가지고 축중합에 의해 합성하였다. 모든 단량체와 고분자는 원소분석, FT-IR, $^1$H-NMR의 분광학적 측정을 통해 정량 정성분석을 행하였다. UV lithography 방법을 사용하여 금 기판 위에 제조한 감광성 폴리이미드 LB 필름의 마이크로 어레이 패턴을 제조하였다. 형성된 마이크로 어레이 패턴을 따라 두 가지의 자기조립 방법으로 단백질 cytochrome c 단분자 막을 고정화시켰다. 자기조립된 cytochrome c 단분자 막의 물리ㆍ전기 화학적 특성은 cyclic voltammetry와 AFM을 통해 조사하였으며 생물전자소자로의 응용 가능성에 대해서도 검토하였다.

Structural Characterization of Physiologically Active Polysaccharides from Natural Products (Arabidopsis)

  • Shin, Kwang-Soon;Darvill, Alan G.
    • Food Science and Biotechnology
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    • 제15권3호
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    • pp.447-452
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    • 2006
  • To determine the functions of specific cell wall polysaccharides, polysaccharides of three mutants, mur3-1, mur3-2, and mur3-3, obtained from Arabidopsis wild type, underwent structural characterization. Upon sequential separation of pectins (RG-I and RG-II) and cross-linking glycans (xyloglucan, XG), only XG was affected by the mud mutation. Wild-type XG contained a considerable amount of fucose, whereas the fucose level in mur3 XGs was less than 20% that of wild type. Further analysis of XGs by matrix-assisted laser-induced/ionization time-of-flight (MALDI-TOF) mass spectrometry indicated that mud lines considerably or completely lost the fucosylated XG oligosaccharides such as XXFG and XLFG and the double-galactosylated oligosaccharide XLLG $^1H$-NMR spectroscopic analyses of the XG oligosaccharides from mur3-3 plant revealed the absence of fucose and a galactose level in the galactosylated side chain that was reduced by 40% compared to that of Arabidopsis wild-type plant. In contrast, 85% less fucose and a slight loss of galactose were observed in the mur3-1 and mur3-2 lines which show normal growth habit. Of the three Arabidopsis mur3 lines studied here, mur3-3 is disrupted by a T-DNA insertion in the exon of MUR3 which encodes XG-specific galactosyltransferase, and exhibits slight dwarfism. These results indicated that the T-DNA insertion at the MUR3 locus did not induce the complete loss of galactose in XG, and that galactose, rather than fucose, in the XG side chains made a major contribution to overall wall strength.

S,S-prodien(=1,9-bis(S)-prolyl-1,9-dioxo-2,5,8-triazanonane)의 입체특이성 반응(I); ${\wedge}-{\alpha}{\beta}$(ffm)-[Co(S,S-prodien)$H_2O$]$ClO_4$의 합성 (Stereospecific Reaction of S,S-prodien(= 1,9-bis(S)-prolyl-1,9-dioxo-2,5,8-triazanonane) (Ⅰ); Synthesis of ${\wedge}-{\alpha}{\beta}$(ffm)-[Co(S,S-prodien)$H_2O$]$ClO_4$)

  • 이배욱;김진우;이동진;김봉곤;오창언;도명기
    • 대한화학회지
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    • 제41권9호
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    • pp.465-470
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    • 1997
  • 입체특이성 반응을 나타내는 키랄성 다섯자리 리간드, 1,9-bis(S)-prolyl-1,9-dioxo-2,5,8-triaza-nonane(S,S-prochen)를 S-proline과 diethylenetriamine (dien)으로부터 합성하여 $^{13}C-NMR$스펙트럼으로 확인하고, $CoCl_2{\cdot}6H_2O$와 반응시켜 적자색의 착물인 $[Co(SS-prodien)H_2O]ClO_4$ 를 합성하였다. 원소분석, 전자흡수스펙트럼, $^{13}C-NMR$스펙트럼 자료에 따라 S,S-prodian은 5자리로 배위되면서 중심의 dien부분은 fac형태로 결합하고, 한자리 리간드인 $H_2O$는 dien에 있는 2차질소원자에 대하여 cis 위치에 존재하는 ${\alpha}{\beta}$ (ffm)-형임을 알게되었다. 또한 CD스펙트럼에 따라 킬레이트된 리가드는 입체선택적으로 배위되어 ${\Lambda}$-${\alpha}{\beta}$ (ffm)-$[Co(SS-prodien)H_2O]^+$의 절대구조를 갖는다고 생각하였다.

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실란 커플링제에 의해 표면이 개질된 실리카 나노입자의 분광학적 분석 (Spectroscopic Analysis of Silica Nanoparticles Modified with Silane Coupling Agent)

  • 송성규;김정혜;황기섭;하기룡
    • Korean Chemical Engineering Research
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    • 제49권2호
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    • pp.181-186
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    • 2011
  • 본 연구에서는 실리카 나노 입자의 표면 개질을 위해 실란 커플링제인 3-(trimethoxysilyl)propylmethacrylate(MPS) 를 사용하여 표면 개질 반응을 수행하였다. 용매의 pH, MPS의 가수 분해 반응시간, 표면 개질 반응시간 및 실리카 표면의 실라놀기(Si-OH)에 대한 MPS의 몰 비를 변화하여 각각의 반응조건이 실리카 표면개질 반응에 미치는 영향을 연구하였다. 개질반응 후 Fourier Transform Infrared Spectroscopy(FTIR), 원소분석(EA) 및 고체 상태 cross-polarization magic angle spinning(CP/MAS) Nuclear Magnetic Resonance Spectroscopy(NMR)법을 사용하여 표면이 개질된 실리카 입자들의 분석을 수행하였다. 연구 결과 용매의 pH가 4.5일 때 MPS가 단량체 형태로 실리카 표면의 실라놀기와 반응하고 이외의 pH에서는 MPS가 이량체, 삼량체 혹은 사량체의 올리고머 형태로 실리카의 실라놀기와 반응함이 우세함을 나타내었다. 가수분해반응 시간을 30분에서 90분으로 증가시키면 MPS가 올리고머 형태로 실리카 표면의 실라놀기와 반응하는 것이 우세하고, 투입한 MPS 몰 비의 증가도 MPS가 올리고머 형태로 실리카 표면의 실라놀기와 반응하는 것이 우세함을 나타내었다.

Interaction Studies of a Novel, Water-Soluble and Anti-Cancer Palladim(II) Complex with Calf Thymus DNA

  • Mansouri-Torshizi, H.;Saeidifar, M.;Divsalar, A.;Saboury, A.A.;Shahraki, S.
    • Bulletin of the Korean Chemical Society
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    • 제31권2호
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    • pp.435-441
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    • 2010
  • We report the preparation and characterization of a new and water soluble complex of palladium(II) with 1,10- phenanthroline and butyldithiocarbamate ligands. This compound has been studied through spectroscopic techniques, $^1H$ NMR, IR, electronic spectra and elemental analysis and conductivity measurements. The complex shows 50% cytotoxic concentration ($Ic_{50}$) value against chronic myelogenous leukemia cell line, K562, much lower than that of cisplatin. Thus the mode of binding of this complex to calf thymus DNA have been extensively investigated by isothermal titration UV-visible spectrophotometry, fluorescence, gel filteration and other methods. UV-visible studies show that the complex exhibits cooperative binding with DNA and remarkably denatures the DNA at extremely low concentration ($~13\;{\mu}M$). Fluorescence studies indicate that the complex intercalate into DNA. Gel filtration studies suggest that the binding of Pd(II) complex with DNA is strong enough that it does not readily break. In these interaction studies, several thermodynamic and binding parameters are also determined which may reflect the mechanism of action of this type of compound with DNA.

Symmetric Bis-Azospiropyrans: Synthesis, Characterization and Colorimetric Study

  • Nourmohammadian, Farahnaz;Abdi, Ali Ashtiani
    • Bulletin of the Korean Chemical Society
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    • 제34권6호
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    • pp.1727-1734
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    • 2013
  • Synthesis and characterization of some novel symmetric bis-azospiropyrans are reported in this study. These bis-azospiropyrans are bifunctional chromophores with two spiropyrans linked by a bis-azo extended aromatic system that produce more color strength (large molar absorption coefficient in mero forms) due to appending two azospiropyran chromophores on one molecule. Comparing to the molar absorption coefficients of the conventional spiropyran chromophores (${\varepsilon}=0.31{\times}10^4\;M^{-1}{\cdot}cm^{-1}$) and mono-azospiropyran chromophores ($1.35{\times}10^4\;M^{-1}{\cdot}cm^{-1}$), the novel synthesized photochromes showed astonishingly increased molar absorption coefficients ($2.3-3.8{\times}10^4\;M^{-1}{\cdot}cm^{-1}$) at the same conditions. Such high molar absorption coefficients confers high sensitivity to light and more color intensity of mero form, that leads to improvement of their light sensitivity and better discrimination of spiro (OFF) form from mero (ON) ones in molecular switches. The structures were deduced from their MS, FT-IR, and $^1H$-NMR spectroscopic data and CHN analysis. All the synthesized photochemically bifunctional compounds revealed fluorescent emission in their colorless form which was faded out after exposing to UV light. Fluorescence quantum yield values of the mero forms were 0.25-0.81 and two high fluorescence quantum yield values (0.60 and 0.81) were found in these series.

Two New Flavonoids from Dragon's Blood of Dracaena cambodiana

  • Mei, Wen-Li;Luo, Ying;Wang, Hui;Shen, Hai-Yan;Zeng, Yan-Bo;Dai, Hao-Fu
    • Bulletin of the Korean Chemical Society
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    • 제34권6호
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    • pp.1791-1794
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    • 2013
  • Phytochemical investigation on dragon's blood of Dracaena cambodiana led to the discovery of two new flavonoid derivatives, cambodianin G (1) and cambodianin H (2). Their structures were elucidated on the basis of detailed spectroscopic analysis, including 1D and 2D NMR techniques and chemical methods. The two compounds were observed to exhibit antibacterial activities against Staphylococcus aureus, and compound 1 showed cytotoxicities against K562 and SGC-7901 cell lines.

산국의 잎과 줄기에서 분리한 Sesquiterpene Lactone들의 구조규명 및 생리활성 (Structural Analysis and Biological Activities of Sesquiterpene Lactones Isolated from the Leaves and Stems of Chrysanthemum boreale Makino)

  • 이종록;박문기
    • 한국환경과학회지
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    • 제26권11호
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    • pp.1285-1295
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    • 2017
  • Chrysanthemum boreale Makino is widely distributed in Korea, China, Japan and Southeast Asian countries. C. boreale is one of the herbs used for treating various inflammatory diseases in oriental medicine. The present study was conducted to identify biologically active compounds from the leaves and stems of C. boreale. We isolated two sesquiterpene sactones from the leaves and stems of C. boreale using silica gel column chromatography and recyclic high perfomance liquid chromatography. The lactones were characterized by their spectroscopic data (NMR, IR, MASS). These compounds were subjected to Farnesyl Protein Transferase (FPTase) inhibition, Nitric Oxide (NO) release inhibition and apoptosis inhibition. The structur of the following isolated compound were elucidated 8,10-${\small{O}$-Acetyl-2-methoxy-10-hydroxy-3,11(13)-guaiadiene-12,6-olide and 4,10-dihydroxy-8-${\small{O}$-Acetyl-2,11(13)-guaiadiene-12,6-olide. In the NO release inhibition assay, compound 2 showed strong activities, with an $IC_{50}$ value of $7{\mu}g/mL$, whereas compound 1 did not exhibit significant activity with an $IC_{50}$ value of over $14{\mu}g/mL$ against murine macrophage.

A New Flavonol Glycoside from Tristemma hirtum (Melastomataceae)

  • Kenfack, Joseph Nandjou;Ponou, Beaudelaire Kemvoufo;Kuhlborn, Jonas;Teponno, Remy Bertrand;Nono, Raymond Ngansop;Fouedjou, Romuald Tematio;Opatz, Till;Park, Hee Juhn;Tapondjou, Leon Azefack
    • Natural Product Sciences
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    • 제24권3호
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    • pp.213-218
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    • 2018
  • Chemical investigation of the plant Tristemma hirtum P. Beauv (Melastomataceae) resulted to the isolation of a new flavonol glycoside named quercetin-7-O-${\alpha}$-D-arabinofuranoside (1), together with nine known compounds including 3'-hexadecanoyl-2'-(9aZ)-tetradecanoyl-glycerol 1'-O-[${\beta}$-D-galactopyranosyl-(1'' ${\rightarrow}$ 6'')-${\alpha}$-D-galactopyranoside] (2), arjunolic acid (3), ${\beta}$-sitosterol-3-O-${\beta}$-D-glucopyranoside (4), terminolic acid (5), quercetin (6), asiatic acid (7), maslinic acid (8), $1{\beta}$-O-galloylpedunculagin (9) and 6-hydroxyapigenin 7-O-${\beta}$-D-glucopyranoside (10) from the methanol extract using normal and reversed phase column chromatography. The structures of these compounds were determined by comprehensive interpretation of their spectral data mainly including 1D- 2D-NMR ($^1H-^1H$ COSY, HSQC, and HMBC) spectroscopic and ESI-TOF-MS mass spectrometric analysis.