• 제목/요약/키워드: $^2H$ NMR

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물오리나무 수피의 Diarylheptanoid (Diarylheptanoids from Bark of Alnus hirsuta Turcz)

  • 황병호;조재현;이태성;배영수
    • Journal of the Korean Wood Science and Technology
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    • 제37권1호
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    • pp.73-77
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    • 2009
  • 본 연구는 우리나라 전역에 분포하고 있는 물오리나무의 추출성분으로부터 유용한 항산화 물질을 탐색하기 위해 수행되었다. 물오리나무 수피를 70% acetone 수용액으로 추출하여 분획한 후 ethyl acetate 분획과 수용성 분획을 Sephadex LH-20으로 충진된 column으로 chromatography를 수행하여 혼합물을 정제하고 두 개의 diarylheptanoid 화합물을 얻었다. 단리된 화합물은 $^1H$, $^{13}C$-NMR 및 2D-NMR 분석을 통하여 1,7-bis-(3,4-dihydroxyphenyl)-heptane-3-one-5-O-${\beta}$-D-xylopyranoside (1, oregonin)와 1,7-bis-(3,4-dihydroxyphenyl)-heptane-5-O-${\beta}$-D-xylopyranoside (2)로 구조를 규명하였다. 두 개의 diarylheptanoid 화합물과 oregonin 가수분해물에 대한 항산화 활성(DPPH)을 측정한 결과 세 화합물 모두 높은 활성을 보였으며, 특히 oregonin 가수분해물의 항산화 활성은 $IC_{50}$이 2.6으로 높은 활성을 보였다.

Solid State Dynamic Nuclear Polarization of 1H Nuclear Spins at 0.3 T and 4.2 K

  • Shim, Jeong Hyun
    • 한국자기공명학회논문지
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    • 제21권4호
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    • pp.114-118
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    • 2017
  • Here, I report solid state Dynamic Nuclear Polarization (DNP) of $^1H$ nuclear spins at 0.3 T and 4.2 K. The DNP polarizer was developed based on a commercial X-band Electron Spin Resonance (ESR) modified for DNP, in combination with a NMR console and a liquid-Helium cryostat. By detuning magnetic field, DNP spectrum was measured to find the optimal condition. At +3 mT detuned from on-resonance field, $^1H$ NMR signal of 60:40 glycerol/water frozen solution doped with 20 mM perdeuterated-Tempone was amplified 43 times. The $^1H$ spin polarization obtained at 4.2 K is over 3100 times higher than that at 300 K. The width of the DNP spectrum, which is five times broader than ESR spectrum, is inconsistent with solid effect or thermal mixing, and presumably suggests a different DNP mechanism.

Synthesis, Spectral Characterization, Electron Microscopic Study and Influence on the Thermal Stability of Phosphorus-containing Dendrimer with a 4,4'-Sulphonyldiphenol at the Core

  • Dadapeer, Echchukattula;Rasheed, Syed;Raju, Chamarthi Naga
    • Bulletin of the Korean Chemical Society
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    • 제32권2호
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    • pp.498-502
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    • 2011
  • The divergent synthesis of novel phosphorus-containing dendrimer with 4,4'-sulphonyldiphenol at the core has been accomplished involving simple condensation reactions using $P(O)Cl_3$, $P(S)Cl_3$, 3-amino-phenol, 3-hydroxy-benzaldehyde, and 2-butyn 1, 4-diol. The final compound was a Schiff's base macromolecule possessing 4 imine bonds, 8 acetylenic bonds and 8 OH groups at the periphery. The structures of intermediate compounds were confirmed by IR, NMR ($^1H$, $^{13}C$ and $^{31}P$), LC-Mass and C, H, N analysis. The structure of the final dendrimer (5) was confirmed by IR, NMR ($^1H$, $^{13}C$ and $^{31}P$), MALDI-TOF-MS, and C, H, N analysis. The surface morphological characteristics of the final dendrimer were understood by Scanning Electronic Microscopic study (SEM). The thermal stability of the final dendrimer was studied by TGA/DTA analysis.

Design, Synthesis, Fluorescence Properties and Antibacterial Activities of New 8-Chloro-3-Alkyl-3H-Pyrazolo[4,3-a]acridine-11-Carbonitriles

  • Rahmani, Zeynab;Pordel, Mehdi;Davoodnia, Abolghasem
    • Bulletin of the Korean Chemical Society
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    • 제35권2호
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    • pp.551-556
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    • 2014
  • The treatment of alkylated nitro derivatives of indazole with 2-(4-chlorophenyl)acetonitrile under basic conditions gave the new 8-chloro-3-alkyl-3H-pyrazolo[4,3-a]acridine-11-carbonitriles via the nucleophilic substitution of hydrogen which proceeds at room temperature with concomitant cyclisation in fairly good yields. The structures of all newly synthesized compounds were confirmed by IR, $^1H$ NMR, $^{13}C$ NMR and mass spectral data. Fluorescence experimental results of all newly synthesized compounds revealed remarkable photoluminescence properties and strong green fluorescence properties. Also, the new compounds exhibited potent antibacterial activity and their antibacterial activity (MIC) against Gram positive (Staphylococcuse aureus methicillin resistant S. aureus and Bacillus subtilis) and negative bacterial (Pseudomonas aeruginosa and Escherichia coli) species were determined.

Structure of an Antimicrobial Peptide Buforin II

  • Yi, Gwan-Su;Park, Chan-Bae;Kim, Sun-Chang;Chaejoon Cheong
    • 한국생물물리학회:학술대회논문집
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    • 한국생물물리학회 1996년도 정기총회 및 학술발표회
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    • pp.29-29
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    • 1996
  • The structure of an antimicrobial peptide buforin II has been studied by $^1$H NMR and CD spectroscopy. Buforin II is flexible and random structure in H$_2$O but the parts of buforin II become helical structure in trifluoroethanol (TFE)/H$_2$O (1:1, v/v) solution. From the restrained molecular dynamics calculation using NMR data, we obtained the possible conformation of buforin II in TFE/H$_2$O solution. (omitted)

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(2-(6-Methyl-2-P-tolyl-lH-imidazo[1,2-a]pyridin-3-yl)핵종을 가지고 있는 불소화된 아조화합물의 합성과 항균활성의 스크리닝 (Synthesis and Antimicrobial Screening of Some Fluorinated Azoles Containing (2-(6-Methyl-2-P-tolyl-lH-imidazo[1,2-a]pyridin-3-yl) Nucleus)

  • Shelke, Sharad;Salunkhe, Nilesh;Sangale, Sandeep;Bhalerao, Swapnil;Naik, Nilesh;Mhaske, Ganesh;Jadhav, Ranjana;Karale, Bhausaheb
    • 대한화학회지
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    • 제54권1호
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    • pp.59-64
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    • 2010
  • 일련의 불소화된 티아디아졸 3, 트리아졸 4, 그리고 옥사디아졸 5이 (2-(6-Methyl-2-P-tolyl-lH-imidazo[1,2-a]pyridin-3-yl)핵종을 가지고 있는 티오세미카르바지드로 부터 합성되어진다. 초음파조사 방법 뿐만 아니라 일반적인 방법에 의해 반응이 진행되었다. 모든 생성물들은 IR, 1H NMR, MS로 구조가 결정되었고, 이들 화합물의 항균활성을 스크닝하였다.

Molecular Motions of [N(C2H5)4]+ and [N(CH3)4]+ ions by 1H Nuclear Magnetic Resonance Relaxation in [N(C2H5)4]2CoCl4 and [N(CH3)4]2CoCl4 Single Crystals

  • Yoon, Su-A;Lim, Ae-Ran
    • 한국자기공명학회논문지
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    • 제15권2호
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    • pp.146-156
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    • 2011
  • The line widths and spin-lattice relaxation times of protons in $[N(C_2H_5)_4]_2CoCl_4$ and $[N(CH_3)_4]_2CoCl_4$ single crystals were investigated in the temperature range 160-400 K. The temperature dependences of the spin-lattice relaxation times are attributed to the molecular motions of the ethyl and methyl groups in the $[N(C_2H_5)_4]^+$ and $[N(CH_3)_4]^+$ ions respectively. The NMR line widths indicate that the ethyl groups in $[N(C_2H_5)_4]_2CoCl_4$ have one more degree of freedom than the methyl groups in $[N(CH_3)_4]_2CoCl_4$. The experimental results are interpreted in terms of the reorientations of the methyl and ethyl groups.

핵자기공명 현미영상법을 이용한 약물전달체계의 비파괴연구 (Noninvasive study of Drug Delivery Systems using Nuclear Magnetic Resonance Microimaging)

  • 이동훈;고락길
    • 대한의용생체공학회:의공학회지
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    • 제18권2호
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    • pp.173-178
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    • 1997
  • pH sensitive polymers have long been utilized as one important type among many interesting drug delivery systems. This is due to the reason of different pH environments in human organs, which requires different pH control mechanism depending upon the organs. In the present study the pH sensitivity was investigated for both pH sensitive and pH insensitive biopolymers using the diffusion effect along with the swelling effect. NMR microscopy was performed along with optical microscopy. For the analysis of diffusion effect, UMR Microscopy was perFormed to measure diffusion coefficients for various liquids such as distilled water, acetone and DMSO(dimethyl sulfoxide). Also, this technique is expected to contribute to the studies for many pH drug delivery systems.

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Synthesis and Characterization of Bis(5,6-dihydro-1,4-dithiin-2,3-dithiolato)nickel(II), nickel(III) and of Related Dialkyl Nickel(III) Dithiolene Complexes

  • 김영진;최성낙;오영희
    • Bulletin of the Korean Chemical Society
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    • 제18권9호
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    • pp.1022-1028
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    • 1997
  • The reaction between Ni(Ⅱ) and sodium salt of 5,6-dihydro-1,4-dithiin-2,3-dithiolate (DDDT2-) in the presence of oxygen results in the formation of Ni(Ⅲ) species, Ni(DDDT)2-, which is isolated as tetraalkylammonium salt. The same reaction performed in the absence of oxygen yields dianionic Ni(Ⅱ) species, Ni(DDDT)22-, which is also isolated as the tetraethylammonium salt. The bis(5,6-dihydro-1,4-dithiin-2,3-dithiolato) nickelate (Ⅱ) dianion, Ni(DDDT)22-, reacts with methyl iodide to yield unusually stable bis(methylthio)dithiolene complex, Ni(CH3)2C8H8S8. All the isolated dithiolato-nickel(Ⅱ) and nickel(Ⅲ) complexes are characterized by 1H NMR, UV/Vis, IR and mass spectroscopic methods. The internal redox reaction of the nickel(Ⅱ)-dithiolate has been studied by spectro-electrochemical method and the results were compared with those of other metal-dithiolenes. The alkylated nickel(dithiolene) complex presumably undergoes cis-trans isomerization reaction in solution, judging from the experimental results of variable-temperature 1H NMR measurements.

$^{11}B$ Nuclear Magnetic Resonance Study of Calcium-hexaborides

  • Mean, B.J.;Lee, K.H.;Kang, K.H.;Lee, Moo-Hee;Lee, J.S.;Cho, B.K.
    • 한국자기공명학회논문지
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    • 제7권2호
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    • pp.80-88
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    • 2003
  • We have performed $^{11}$ B nuclear magnetic resonance (NMR) measurements to microscopically investigate an electronic structure of the ferromagnetic state in three different compositions of calcium-hexaboride single crystals. Although the crystal structure of Ca $B_{6}$ is cubic and three NMR lines may be expected for the nuclear spin 3/2 of $_{11}$ B, a larger number of NMR resonance peaks have been observed. The frequency and intensity of those peaks distinctively changes depending on the angle between crystalline axis and magnetic field. Analyzing this behavior, we find that the electric field gradient(EFG) tensor at the boron has its principal axis perpendicular to the six cubic faces with a quadrupole resonance frequency $v_{Q}$ 600 kHz. Even though the magnetization data highlight the ferromagnetic hysteresis, $^{11}$ B NMR linewidth data show no clear microscopic evidence of the ferromagnetic state in three different compositions of Ca $B_{6}$ single crystals.s.

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