• 제목/요약/키워드: Solution NMR

검색결과 565건 처리시간 0.023초

The [M(cod)(PPh$_3)_2] PF_6$ (M = Rh, Ir; cod = 1,5-cyclooctadiene) Mediated Activiation of Aldehyde C-H Bond

  • Ko, Jae-Jung;Joo, Wan-Chul
    • Bulletin of the Korean Chemical Society
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    • 제8권5호
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    • pp.372-376
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    • 1987
  • Acetone solution of quinoline-8-carbaldehyde reacts with $[Rh(cod)(PPh_3)_2] PF_6$and $[Ir(cod)(PPh_3)_2] PF_6$ to yield $[Rh(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (1) and $[Ir(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (2), respectively. The compound $[Ir(cod)(PPh_3)_2] PF_6$ also reacts with $Ph_2PC_6H_4-o-CHO$ in the acetone / $H_2O$ mixture to give $[Ir(Ph_2PC_6H_4-o-CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (3). Compounds 1, 2, and 3 were characterized by infrared, $^1H$ NMR, $^{31}P$ NMR spectra and conductivity measurement. The $^1H$ NMR spectra of 1, 2, and 3 support the presence of a terminal hydride that is cis to the phosphine. The IR band of 3 at 2185 $cm^{-1}$, which is assigned to $\nu$(Ir-H), and the hydride cleavage reaction of 3 with $CCl_4$, provide evidence for the Ir-H bond.

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.

Conformational Characteristics of p-tert-Butylcalix[6]arene Mono-Alkyl Ester Derivatives

  • Yu, Hyo-Yeon;Seok, Da-Hyun;Chang, Suk-Kyu;Ahn, Sang-Doo;Chung, Kee-Choo
    • 한국자기공명학회논문지
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    • 제14권2호
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    • pp.144-153
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    • 2010
  • Conformational properties of several mono-alkyl ester derivatives of p-tert-butylcalix[6]arene depending on temperatures have been investigated by solution NMR spectroscopy. It is found out that all derivatives can adopt a cone-like conformation around room temperature, while the conformational characteristics at high temperatures seem to be quite different each other.

Phenazine Ring을 가진 界面活性劑의 合成과 그 抗菌性 (제1보) (Synthesis and Antimicrobial Properties of Surfactants Containing Phenazine Ring (Ⅰ))

  • 김종대;박영훈
    • 대한화학회지
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    • 제25권3호
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    • pp.199-205
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    • 1981
  • Aniline과 alcohol류에서 4-aminoalkylbenzene을 合性하여, 이것을 아세틸化, 니트로化, 加水分解하여 3-nitro-4-aminoalkylbenzene을 얻고 아미노기 이탈반응을 통해 3-nitroalkylbenzene을 合成하여 anthranilic acid와 반응시켜 7-alkyl-1-carboxyphenazine 유도체를 合成하였다. 生成物은 元素分析, IR, NMR 스펙트럼으로 確認하였다. 이들 誘導體들의 水溶液에 대한 表面張力을 測定하였고, 아울러 Gram 陽性菌, Gram 陰性菌, 眞性菌에 대한 抗菌性을 調査하였다. 試驗結果 alkyl기가 치환된 phenazine 誘導體의 抗菌性은 alkyl기가 없는 1-carboxyphenazine 보다 强한 것으로 나타났다.

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Structural and Dynamic Studies of the Central Segments in the Self-complementary Decamer DNA Duplexes d(ACGTATACGT)2 and d(ACGTTAACGT)2

  • Park, Jin-Young;Lee, Joon-Hwa;Choi, Byong-Seok
    • BMB Reports
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    • 제31권1호
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    • pp.89-94
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    • 1998
  • The structures of the self-complementary decamer duplexes, $d(ACGTATACGT)_2$ (TATA-duplex) and $d(ACGTTAACGT)_2$, (TTAA-duplex) has been obtained in solution by proton NMR spectroscopy and restrained molecular dynamics. The duplexes are essentially B-type, with distortions apparent at the TATA and TTAA steps. Theses distortions and their effects on dynamics have been investigated by the measurement of imino proton exchange time of the base-pairs. The unusual opening kinetics of central A T base-pairs could be correlated to the abnormal structural properties of the corresponding sequences.

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Conformation of Substance P in Neutral Phospholipid Micelles

  • Kim, Seonggeum;Eunjung Bang;Kim, Yangmee
    • 한국자기공명학회논문지
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    • 제2권1호
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    • pp.41-49
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    • 1998
  • A linear undecapeptide, Substance P (SP) is involved in a wide variety of physiological processes such as pain, inflammation, salivation, and hypertension. Tertiary structure of SP in dodecylphosphocholine (DPC) micelles has been investigated by CD, NMR spectroscopy, and DGII calculation. CD spectrum of SP in the presence of 7.5 mM DPC micelles does not show any favorable secondary structure. The tertiary structure determined by NMR spectroscopy and DGII calculation shows that the Phe7-Phr8-Gly9-Leu10 region adopts a turn structure, while the N-terminal region is quite flexible. Both prolines in SP exist preferentially as the trans isoforms and the aromatic ring of Phe7 protrudes outward. Conformation of SP may be restrained by the contact of the Phe7 aromatic ring with the hydrophobic side chains of the DPC micelles and this interaction induces a turn structure. Structure of SP in aqueous solution in the presence of DPC micelles can represent a good model to study the conformation recognized by the receptor near neutral membrane.

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Separation and Purification of Useful Proteins Using Hydrogel Ultratiltration

  • Park, Chang-Ho;Son, Chang-Kyu;Park, Jong-Hwa;Chung, In-Sik
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제2권2호
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    • pp.113-116
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    • 1997
  • The hydrogel process is a different form of ultrafiltration and has been used to separate biological molecules. In this study, the gel pore size was predicted by pulse NMR technique and neural network using a database obtained from gel filtration chromatography and diffusion experiment. Recombinant alkaline phosphatase expressed in insect cells was concentratred 1.5 times by hydrogel ultrafiltration by swelling at 2$0^{\circ}C$ and collapsing at 35$^{\circ}C$ at 53-65% separation efficiency and 78-83% enzyme recovery. Wild and recombinant Autographa californica unclear polyhedrosis viruses (AcNPV) were also concentrated 1.4 and 1.6 times of the feed solution at 48.5 and 60.0% separation efficiency, respectively Hydrogel ultrafiltration appears to be an attractive alternative for the concentration of AcNPV and recombinant proteins from insect cells.

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Synthesis and Characterization of Poly(fluorenylenevinylene-terphenylenevinylene) Containing Phenyl Pendant Group

  • Kim Yun-Hi;Jung Sung-Ouk;Lee Kwang-Hoi;Kwon Soon-Ki
    • Macromolecular Research
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    • 제14권1호
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    • pp.81-86
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    • 2006
  • Poly(fluorenylenevinylene-terphenylenevinylene) containing phenyl pendant group was synthesized by Suzuki coupling reaction and characterized by ${1}^H$-NMR, ${13}^C$-NMR, and IR-spectrum. The weight average molecular weight ($M_{w}$) of the obtained polymer was 31,000 with a polydispersity index of 1.9. The polymer showed good solubility in common organic solvents, and the solution and film emitted blue emission ($\lambda_{max}$=460 nm) on irradiation with UV light. The ITO/PEDOT/polymer/Al device fabricated using the polymer as an emitting layer emitted blue light with a maximum peak around 460 nm. The maximum efficiency of the device was 0.011$\%$.

SOLUTION STRUCTURE AND INTERACTION ON THE CARBOXYL- TERMINAL DOMAIN OF ESCHERICHIA COLI RNA POLYMERASE $\alpha$ SUBUNIT STUDIED BY NMR

  • Jeon, Young-Ho;Tomofumi Negishi;Masahiro Shirakawa;Toshio Yamazaki;Nobuyuki Fujita;Akira Ishihama;Yoshimasa Kyogoku
    • 한국생물물리학회:학술대회논문집
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    • 한국생물물리학회 1996년도 정기총회 및 학술발표회
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    • pp.11-11
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    • 1996
  • The three-dimensional structure of the carboxyl-terminal domain of the E.coli RNA polymerase $\alpha$ subunit, which is regarded as the contact site for transcription activator proteins and the promoter UP element, was determined by NMR spectroscopy. Its compact structure of four helices and two long arms enclosing its hydrophobic core shows a folding topology distinct from those of other DNA-binding proteins. (omitted)

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NMR STRUCTURE DETERMINATION OF A NOVEL CONOTOXIN, [Pro 7,13] $\alpha$A-conotoxin $P_{IVA}$

  • Han, Kyou-Hoon;Hwang, Kae-Jung;Kim, Seung-Moak;Kim, Soo-Kyung;William R. Gray;Shon, Ki-Joon;Jean Rivier;Baldomero M. Olivera
    • 한국생물물리학회:학술대회논문집
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    • 한국생물물리학회 1996년도 정기총회 및 학술발표회
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    • pp.10-10
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    • 1996
  • High-resolution solution conformation of a novel conotoxin, [Pro 7,13] $\alpha$A-conotoxin $P_{IVA}$, GCCGSYPNAACHPCSCKDROSYCGQ-N $H_2$, has been determined by two-dimensional $^1$H nmr methods in combination with distance geometry calculation to rmsd values of 0.90 $\AA$ and 1.16 $\AA$ for the backbone and heavy atoms, respectively. Total of 324 NOE-derived interproton distance restraints including 33 long-range NOE restraints a well as 11 $\Phi$ and 7 $\chi$$^1$ torsion angle restraints were used for computation of structures. (omitted)d)

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