• 제목/요약/키워드: $^1H$ NMR

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$^1H$ NMR Study of Imidazole, L-Histidine, and Their Derivatives Coordinated to the Paramagnetic Undecatungstocobalto(II)silicate and -nickelo(II)silicate Anions

  • Moonhee Ko;Gyung Ihm Rhyu;Hyunsoo So
    • Bulletin of the Korean Chemical Society
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    • v.15 no.8
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    • pp.673-679
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    • 1994
  • $^1H$ NMR spectra of imidazole, 2-and 4(5)-methylimidazole, histamine, L-histidine, L-histidine methyl ester, N${\alpha}$-acetyl-L-histidine, and L-carnosine coordinated to the paramagnetic undecatungstocobalto(II)silicate ($SiW_{11}Co$) and undecatungstonickelo(II)silicate ($SiW_{11}Ni$) anions are reported. For these complexes the ligand exchange is slow on the NMR time scale and the pure resonance lines of the free ligand and the complexes have been observed separately at room temperature. Two different complexes are formed, depending upon which nitrogen atom of the imidazole ring is coordinated to the cobalt or nickel ion of $SiW_{11}M$. Thus the NMR spectrum of a $D_2O$ solution containing a ligand and $SiW_{11}M$ consists of three sets of lines originating from the free ligand and two complexes. All NMR lines of the $SiW_{11}Co$ complexes have been assigned unequivocally using the saturation transfer technique. The temperature dependence of some spectra are also reported. The NMR spectra of some complexes show that the internal rotation of the substituent on the imidazole ring is hampered by the heteropolyanion moiety even at room temperature.

Syntheses and Spectroscopic Studies of [$Cp_2ZrR]_2Fe(CO)_4$

  • Ko, Jae-Jung
    • Bulletin of the Korean Chemical Society
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    • v.7 no.6
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    • pp.413-421
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    • 1986
  • Hydrocarbon solution of $Cp_2Zr(CH_3)Cl$ react rapidly with $Na_2Fe(CO)_4$ (1/2 equiv.) to yield $[Cp_2Zr(CH_3)]_2Fe(CO)_4$ and NaCl. The more soluble metal-metal bonded complex $[Cp_2ZrC_8H_{17}]_2Fe(CO)_2$ has also been prepared through the reaction of $Cp_2Zr(C_8H_{17})BF_4$ and $Na_2Fe(CO)_4 (1/2 equiv.). The complexes were characterized by IR, $^1H$ NMR, ^{13}C$ NMR, and elemental analysis. The infrared spectrum of $[Cp_2ZrR]_2Fe(CO)_4$ shows four bands, which is indicative of a cis-structure. The $^{13}C$ NMR spectrum provides evidence for the cis-structure.

$^1H$ NMR Study of 4-Aminopyrimidine Coordinated to the Paramagnetic Undecatung-stocobalto(Ⅱ)silicate Anion: Rates of Internal Rotation of the Amine Group

  • 김병안;소현수
    • Bulletin of the Korean Chemical Society
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    • v.20 no.10
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    • pp.1149-1152
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    • 1999
  • 1H NMR spectrum of a DMF-d7 solution containing 4-aminopyrimidine and [SiW11CoIIO39]6- (SiW11Co) shows separate peaks from two linkage isomers, a and b, in which N(1) and N(3) of the pyrimidine ring are coordinated to SiW11Co, respectively. The signal from the amine group in the isomer a exhibits temperature dependence that is characteristic of a two-site exchange problem. Rates of internal rotation of the amine group were determined by simulating the NMR spectra at 5-35℃. The amine group of free 4-aminopyrimidine also shows temperature-dependent spectra at lower temperatures; rates of internal rotation at (-25)-25℃ were determined. The internal rotation of the amine group in the complex is much slower than that for free 4-aminopyrimidine, indicating that π-character of the C-N bond increases on coordination to SiW11Co. The amine group in the isomer b does not show such behavior. It is probable that hydrogen bonding between N-H and a bridging oxygen atom of SiW11Co prevents it from rotating at low temperatures.

The Solubilization Site of Some Phenyl Alkanols in Aqueous Sodium Dodecylsulfate Micelle (몇가지 페닐 알카놀의 Sodium Dodeylsulfate 수용액 미셀내에서의 가용화 위치)

  • Jeong, Jong Jae;Gang, Jeong Bu;Lee, Gyeong Hui
    • Journal of the Korean Chemical Society
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    • v.38 no.3
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    • pp.194-199
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    • 1994
  • The solubilization sites of some phenyl alkanols such as phenol, benzyl alcohol, phenethyl alcohol, 3-phenyl-1-propanol solubilized in 0.2 M aqueous sodium dodecylsulfate micelle solution was studied by two dimensional heteronuclear correlation spectroscopy (2D C-H COSY). The results show more quantitative and clear solubilization sites in the SDS micelle than previous results using $^1H$-NMR spectrum integration. We found that most of the phenyl alkanols penetrate into the core of SDS micelle, and the insertion depth was 6.5∼7.0 methylene units from ${\alpha}$-methylene.

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Studies on Chemical Structure Determination of Polygonatum sibiricum Extracts(I) (황정(黃精) 추출물의 화학구조 결정에 관한 연구(I))

  • 신동수;윤중호;박주희;권기락;안철진;주우홍;강진호;문병호
    • Journal of Life Science
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    • v.9 no.2
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    • pp.207-211
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    • 1999
  • Biologically active compounds in Polygonatum sibiricum were extracted using organic solvents as hexane, CHCl$_3$, n-butanol corresponding each component. Compound I was purified from hexane layer and the chemical structure of compound I was characterized using 1H-NMR, 13C-NMR, DEPT135, COSY, HMQC, HMBC spectrum and MS-spectrum. Consequently, the chemical structure of compound I was determined as 9,12-(9E,l2E)-octade cadienoic acid.

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Effective Synthesis of $\alpha$--Bromo-$\omega$ -fluoroalkane with Analysis of Gas-chromatography (가스크로마토그라피 분석을 통한 $\alpha$-브로모-$\omega$ -플루오로알칸의 효율적 합성)

  • Yu, Kook Hyun
    • Journal of the Korean Chemical Society
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    • v.39 no.5
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    • pp.414-420
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    • 1995
  • $\alpha$-Bromo-$\omega$-fluoroalkanes are synthesized in 19∼55% yields from the reactions of dibromoalkanes with AgF and TBABr in acetonitrile at $82^{\circ}C$ for 20 minutes. The reaction is monitored with gas-chromatography. 1^H$ NMR and $19^F$ NMR-Spectrometer are used for identification of $\alpha$-Bromo-$\omega$-fluoroalkanes, difluoroalkane, fluoroalken and bromoalkene.

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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.2
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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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Influence of Hot Pressing on the Pore Structure of Nafion Electrolyte Membrane Investigated by 1H NMR

  • Jeonga, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1559-1562
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    • 2009
  • The influence of hot pressing on the pore structures of Nafion membranes was investigated by observing the Nafion before and after hot pressing with $^1H$ nuclear magnetic resonance (NMR) spectroscopy. The freezing point depression and chemical shift data of water in the Nafion indicated the presence of two different pore size ranges in Nafion. Hot pressing mainly reduced the sizes and number of the big pores. The reduction of water uptake and proton conductivity after hot pressing was explained by this variation of pore size and number. We demonstrated the potential application of chemical shift data and NMR cryoporometry experiments to measure the relative pore sizes, on a nano scale, and numbers.

Studies on the interaction of thiamines and cyclodextrins

  • Im, In-Seon;Lee, Wang-Kyu;Park, Man-Ki;Kim, Bak-Kwang
    • Archives of Pharmacal Research
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    • v.6 no.1
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    • pp.35-44
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    • 1983
  • Interactions between thiamine.HCl and its disulfide derivatives TTFD. TPD and .alpha., .betha. cyclodextrins were investigated. By measuring the H-NMR, C-NMR chemical shifts, the assumption that cyclodextrin may from a inclusion complex with thiamines was supported qualitatively. To calculated the stability constants of them, anion exchange chromatography was applied. The simple, rapid HPLC method was proved to be pertinent thiamine/cyclodextrin system which was chemically unstable and less soluble.

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Quantification of Allantoin in Yams (Dioscorea sp.) Using a 1H NMR Spectroscopic Method

  • Thao Quyen Cao;Dongyup Hahn
    • Journal of Microbiology and Biotechnology
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    • v.33 no.5
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    • pp.662-667
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    • 2023
  • Allantoin is an abundant component of yams and has been known as a skin protectant due to its pharmacological activities. In previous methods for allantoin determination using high-performance liquid chromatography (HPLC), the separation was unsatisfactory. We herein developed a 1H quantitative nuclear magnetic resonance (qNMR) method for quantification of allantoin in the flesh and peel of yams. The method was carried out based on the relative ratio of signals integration of allantoin to a certain amount of the internal standard dimethyl sulfone (DMSO2) and validated in terms of specificity, linearity (range 62.5-2000 ㎍/ml), sensitivity (limit of detection (LOD) and quantification (LOQ) 4.63 and 14.03 ㎍/ml, respectively), precision (RSD% 0.02-0.26), and recovery (86.35-92.11%). The method was then applied for the evaluation of allantoin in flesh and peel extracts of four different yams cultivated in Korea.