• Title/Summary/Keyword: F NMR

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Synthesis and Anion Binding Affinities of Novel Molecular Tweezers Based on Chenodeoxycholic Acid Bearing Different Lengths of Arm

  • Kim, Ki-Soo;Jang, Hyun-Seok;Kim, Hong-Seok
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1445-1449
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    • 2006
  • Molecular tweezers based on chenodeoxycholic acid bearing different lengths of arm were synthesized andtheir anion binding affinities were evaluated by $^1H$ NMR, isothermal calorimetric titration, and ESI mass spectrometry. Molecular tweezer 6 showed a high selectivity toward $H_2PO_4\;^-$ over $Cl^-,\;Br^-,\;I^-, $ and $CH_3CO_2\;^-$ by $^1H$ NMR titration, whereas the association constant for $F^-$ revealed the largest value as determined by ITC. The selectivity of 6 towards $F^-$ was about 103 times higher than that of $Cl^-,\;H_2PO_4\;^- $, and $CH_3CO_2\;^-$. ITCexperiment of 6 with $F^-$ in a DMSO showed two binding modes; two sequential association constants $K_1\;=\;2.77\;{\times}\;10^5\;M^{-1}$ and $K_2\;=\;8.68\;{\times}\;10^6\;M^{-1}$ were found. These sequential bindings were confirmed by ESI massspectrometry. 1 : 1 and 1 : 2 complexes of 6 and $F^-$ were found at m/z 868.08 and 884.04.

Synthesis and Characterization of Two New Fluoroplumbate(II) Complexes: Tetrabutylammonium Fluorodihaloplumbate, (But)4N[PbX2F] (X = Cl, I)

  • Javanshir, Zahra;Mehrani, Kheyrollah;Ghammamy, Shahriare;Saghatforoush, LotfAli;Seyedsadjadi, Seyedabolfazl;Hassanijoshaghani, Ali;Tavakol, Hossein
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1464-1466
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    • 2008
  • Tetrabutylammonium Fluorodichloroplumbate(II), N$(C_4H_9)_4$[$PbCl_2F$], TBAFDiCP and Tetrabutylammonium Fluorodiiodoplumbate(II), [$(C_4H_9)_4$N][$PbI_2F$], TBAFDiIP are the first examples of fluoroplumbate salts that have been prepared from the reaction of $(C_4H_9)_4$NF with $PbCl_2$ and $PbI_2$ respectively using either $CH_3CN$ solvent. These new compound characterized by elemental analysis, IR, UV/Visible, $^1H$ NMR, and $^{19}F$ NMR techniques.

Studies on Xanthine Oxidase Inhibitor Produced from Aspergillus sp. F184 (Aspergillus sp. F184가 생산하는 Xanthine Oxidase 저해제에 관한 연구)

  • 박시형;윤상웅;박정민;옥승호;유주현;배동훈
    • Microbiology and Biotechnology Letters
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    • v.28 no.2
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    • pp.92-96
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    • 2000
  • Aspergillus sp. F184 was isolated from soil for the development of new xanthine oxidase inhibitor. This xanthine oxidase inhibitor was sequentially purified by filtration, HP-20 adsorption column chromatography, ethyl acetate extraction, silica gel column chromatography and crystallization, and was named as YUX 104. YUX 104 was identified to be 5,6-epoxy-2-hydroxy-3-methyl-2-cyclohexene-1,4-dione(terreic acid) by NMR and mass spectroscopic sudies.

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GERI-BP001 Compounds, New Inhibitors of Acyl-CoA: Cholesterol Acyltransferase from Aspergillus fumigatus F37

  • Jeong, Tae-Sook;Kim, Sung-Uk;Son, Kwang-Hee;Kwon, Byoung-Mog;Kim, Young-Kook;Bok, Song-Hae
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1995.04a
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    • pp.67-67
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    • 1995
  • Acyl-CoA:cholesterol acyltransferase (ACAT, EC 2.3.1.26) plays an important role in the control of intracellular free cholesterol content via its cholesterol esterifying activity. ACAT inhibitors are expected to be effective for treatment of atherosclerosis and hypercholesterolemia. In the course of a screening program for ACAT inhibitors from microbial sources, GERI-BP001 M, A, and B were isolated from the fermentation broth of a fungal strain. GERI-BP001 compounds were isolated from a culture broth of Aspergillus fumigatus F37 by acetone extraction, EtOAc extraction, SiO$_2$ column chromatography, and reverse phase HPLC. The structure of GERI-BP001 coumpounds were determined by $^1$H-NMR, $\^$l3/C-NMR, 2D-NMR, NOESY, and long range C-H COSY experiments. GERI-BP001 M, A, and B inhibit ACAT activity in an enzyme assay system using rat liver microsomes by 50% at concentrations of 75, 147, and 71 ${\mu}$M, respectively.

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$^{13}$C NMR Study of the Application of the 'Tool of Increasing Electron Demand' to the 9-Aryl-tricyclo[3.3.1.0$^{2,8}$]non-9-yl, and 8-Aryl-Tetracyclo[3.2.1.0$^{2,7}$.0$^{4,6}$]oct-8-yl cations

  • Wie-Chang Jin;Gweon-Young Ryu;Chun Yoon;Shin Jung Hyu
    • Bulletin of the Korean Chemical Society
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    • v.10 no.6
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    • pp.591-595
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    • 1989
  • The$^{13}C$ NMR shifts of a series of para-substituted 9-aryl-tricyclo$[3.3.1.0^{2,8}]$non-9-yl and 8-aryl-tetracyclo$[3.2.1.0^{2,7}.0^{4,6}]$-oct-8-yl cations were measured in $FSO_3H/SO_2ClF \;at\; -90^{\circ}C\; or\; -70^{\circ}C$ in order to examine whether the ${\rho}^{c+}$ values can be used to explain the mechanism for the stabilization of the geometrically rigid cyclopropylcarbinyl cations. Plots of the ${\Delta}{\delta}^{c+}$ shifts against ${\sigma}^{c+}$ reveal excellent linear correlation. The tricyclononyl systems yield a ${\rho}^{c+}$ value of -4.95 with a correlation coefficient r = 0.9948. The tetracyclo-octanyl systems give a ${\rho}^{c+}$ value of -6.39 with r = 0.9943. A fair parallelism exists between the results of $^{19}F$ nmr studies and the change of ${\rho}^{c+}$ values in these cations. Accordingly, the present study established that the ${\rho}^{c+}$ value can be used as a mearsure of the geometric influence for the charge delocalization in cyclopropylcarbinyl cations.

$^{13}C-NMR$ Study of the Applicaton of the “ Tools of Increasing Electron Demand ” to the 8-Aryl-tricyclo $[3.2.1.0^{2,7}]$oct-8-yl Cations

  • Gweon-Young Ryu;Jung-Hyu Shin
    • Bulletin of the Korean Chemical Society
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    • v.12 no.2
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    • pp.193-196
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    • 1991
  • The $^{13}C-NMR$ shifts of a series of para-substituted $8-aryl-tricyclo[3.2.1.0^{2,7}]oct-8-yl$ and $9-aryl-tricyclo[3.3.1.0^{2,8}]-non-9-yl$ cations were measured in $FSO_3H/SO_2ClF\ at\-90^{\circ}$ in order to examine whether the ${\rho}^{C^+}$ values can be used as a measure of the geometric influence on the charge delocalization resulting from ${\rho}$ conjugation in rigid tricyclopropylcarbinyl cations. Plot of the ${\Delta}{\delta}^{C+} shifts against the ${\sigma}^{C+}$ constants revealed excellent linear correlation. The 8-aryl tricyclooctyl systems yielded a ${\rho}^{C+}$ value of -5.00 with r = 0.9962. Previous investigation of the 9-aryl-tricyclononyl systems gave a correlation coefficient of r = 0.9948 with a slope of ${\rho}^{C+}$ = -4.95. A fair parallelism exists between the results of $^{19}F-NMR $ studies and the change of ${\rho}^{C+}$ value in these cations. Consequently, it is established that the ${\rho}^{C+}$ value can be used to explain the mechanism of charge stabilization of the rigid cyclopropylcarbinyl cation such as tricyclo $[3.2.1.0^{2,7}]oct-8-yl$ cation.

Preparation and Structure of trans-Bis(tert-butylamine)dichloropalladium(II), trans-[$PdCl_2(t-BuNH_2)_2$] (trans-Bis(tert-butylamine)dichloropalladium(II), trans-[$PdCl_2(t-BuNH_2)_2$의 합성 및 구조)

  • 김혜진;한원석;이순원
    • Korean Journal of Crystallography
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    • v.12 no.1
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    • pp.10-13
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    • 2001
  • Compound PdCl₂(PhCN)₂(1) reacted with tert-butylamine(t-BuNH₂) to give trans-[PdCl₂(t-BuNH₂)₂] (2) Compound 2 was characterized by spectroscopy (¹H-NMR, /sup 13/C{¹H}-NMR, and IR) and X-ray diffraction. Crystallographic data for f2: monoclinic space group p2₁/c, a=6.298(1)Å, b=20.740(2)Å, c=10.731(1)Å, β=92.58(1)°, Z=4, R(wR₂)=0.0207(0.0543).

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A $^{13}C$ NMR Study of 7-Norbornadienyl Cation by Modified Hammett-Brown Equation

  • 박정규;신정휴
    • Bulletin of the Korean Chemical Society
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    • v.20 no.6
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    • pp.667-671
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    • 1999
  • A series of the para-substituted 7-aryl-norbornadienyl cation (3) was prepared in FSO3H/SO2ClF solution at -100℃ and their 13C NMR shifts were measured at -80℃. The plots of the chemical shifts (changes in chemical shifts) of cationic carbon, ΔδC+, aganist our calculated new substituent constant, σc+s, gave an excellent correlation (r=0.994), with a ρc+ value of 12.63. These results indicate that the new substituent constants, σc+s, can be successfully employed to compare the relative charge demand of the carbonium ion by π-and πσ-participation.

Power Absorption Measurements during NMR Experiments

  • Felix-Gonzalez, N.;Urbano-Bojorge, A.L.;de Pablo, C. Sanchez-L;Ferro-Llanos, V.;del Pozo-Guerrero, F.;Serrano-Olmedo, J.J.
    • Journal of Magnetics
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    • v.19 no.2
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    • pp.155-160
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    • 2014
  • The heating produced by the absorption of radiofrequency (RF) has been considered a secondary undesirable effect during MRI procedures. In this work, we have measured the power absorbed by distilled water, glycerol and egg-albumin during NMR and non-NMR experiments. The samples are dielectric and examples of different biological materials. The samples were irradiated using the same RF pulse sequence, whilst the magnetic field strength was the variable to be changed in the experiments. The measurements show a smooth increase of the thermal power as the magnetic field grows due to the magnetoresistive effect in the copper antenna, a coil around the probe, which is directly heating the sample. However, in the cases when the magnetic field was the adequate for the NMR to take place, some anomalies in the expected thermal powers were observed: the thermal power was higher in the cases of water and glycerol, and lower in the case of albumin. An ANOVA test demonstrated that the observed differences between the measured power and the expected power are significant.