• Title/Summary/Keyword: $^{11}$B NMR

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The Synthesis and Characterization of Some Novel Thioethers: Thio-Subsituted [3]Cumulenes, -1-Buten-3-ynes and Buta-1,3-dienes

  • Ibis, Cemil;Sahin, Aysecik
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2255-2260
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    • 2010
  • In this study, some novel thiosubstituted butenyne (3a-d, 7b, 15b), butadiene (4a-b, 4d, 5a, 5c, 6b, 8e, 9c, 10b, 16b, 18e) and [3]cumulene (11a-b with isomer 3a-b, 12a with isomer 13a, 14b, 17e) compounds were synthesized from the reaction of 2H-pentachloro-1,3-butadiene with thiols. The new compounds were characterized by elemental analysis, mass spectrometry, UV-vis, IR, 1H NMR, NMR ($^{13}C$ or APT) spectroscopy.

Constituents of the Herb of Isodon excisus var. coreanus

  • Kim, Ho-Kyoung;Whang, Wan-Kyunn;Kim, Il-Hyuk
    • Archives of Pharmacal Research
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    • v.20 no.3
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    • pp.291-296
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    • 1997
  • The studies were carried out to evaluate the constituents in the aerial part of Isodon excisus var. coreanus (Labiatae). From the aqueous fraction of methanol extract, compound I (${\alpha}$-[[3-(3, 4-dihydroxyphenyl)-1-oxo-2-propenyl]oxy]-3,4-dihydroxy-benzenepropanoic acid), compound II (9-methyl-dihydroferulic acid-4-O-.betha.-D-glucopyranosyl $(1{\rightarrow}2)$-${\alpha}$-L- rhamnopyranosyl (1.rarw.4)-.betha.-D-glucopyranoside), compound III (ent-7.alpha., 11${\alpha}$,15.betha.-trihydroxy-kaur-16-en-1-O-.betha.-D-glucopyranoside) and compound IV ($2{\alpha}$,3${\beta}$,$7{\alpha}$,23-tetrahydroxy-olean-12 -en-28-oic acid 28-O-${\beta}$-D-glucopyranoside) were isolated and identified on the basis of their physicochemical and spectroscopic evidences[IR, FAB(-)MS,$^{1}H-NMR,$$^{13}C-NMR,$$ HMQC$$^{1}H-^{1}H $COSY and HMBC (Heteronuclear Multiple Bond Connectivity)]. Especially, New compounds II and III were named Isodonin A and Isodonin B respectively.

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X-Ray and NMR Studies of Vanadium(V)-Nitrilotriacetate Complex (바나듐(V)-니크릴로트리아세테이트 착물의 X-선 및 핵자기공명 연구)

  • Lee, Man-Ho;Jeong, Woo-Won
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.196-202
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    • 1997
  • New vanadium(V) complex, $(NH_4)_2[VO_2NTA]$, has been synthesized and its structure has been determined by solution and solid-state NMR spectroscopies as well as X-ray crystallography. The unit cell of the monoclinic crystals contains four complexes with $a=6.923(1){\AA}$, $b=8.824(2){\AA}$, $c=19.218(11){\AA}$ and ${\beta}=91.60(3)^{\circ}$ in the space group of $P2_1/n$. The $[VO_2NTA]^{2-}$ anion has distorted octahedral geometry with cis-$VO_2$ moiety. It is confirmed that the octahedral geometry is retained in both of solution and solid-state complexes.

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New Implementation Method of the Pulsed Nuclear Magnetic Resonance Apparatus (펄스방식의 핵자기 공명장치에 관한 새로운 구현방법)

  • 김청월
    • Journal of the Korean Institute of Telematics and Electronics C
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    • v.35C no.10
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    • pp.1-11
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    • 1998
  • This paper presents a new implementation method of the pulsed NMR(nuclear magnetic resonance) apparatus, which contains a single coil in a magnet console, to detect a NMR signal. Applying an RF magnetic field of 5MHz to the magnet console which is designed to have Larmor frequency of 5MHz for hydrogen atom, the hydrogen NMR signal was obtained from the glycerin which was put in the magnet console as a sample. The DC magnetic field in the magnet console was implemented with a permanent magnet of 1168 gauss and the RF magnetic field was generated appling an RF signal with the frequency of 5MHz and the current magnitude of 8A to a coil of 5.73${\mu}$H. The magnitude of the NMR signal was maximum when the RF magnetic field was generated for 2.8 ${\mu}$sec, and the period of generating the RF magnetic field was designed to 100msec for detecting the NMR signal repeatedly. The NMR signal, radiated from the sample in the magnetic console, was appeared as an amplitude-modulated signal with a frequency equal to the Larmor frequency. The signal, induced in the coil, was amplified in the tx/rx separation circuit, preamplifier and intermediate amplifier by a factor of 20.7dB, 36dB and 40dB, respectively, and the signal was detected by a synchronous detection circuits, then the NMR signal was obtained.

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An NMR Study of Solvent Interactions in a Paramagnetic System

  • Golding, R.M.;Pascual, R.O.;Suvanprakorn, C.;Dance, I.G.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1752-1756
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    • 2006
  • This study explores and interprets in a new way the complex solvent and the temperature dependence of the NMR shifts for the N-$CH_2$ protons in tris(N,N-diethyldithiocarbamato) iron(III) in acetone, benzene, carbon disulfide, chloroform, dimethylformamide and pyridine. The NMR shifts are interpreted in terms of the Fermi contact interaction and the dipolar term from the multipole expansion of the interaction of the electron orbital angular momentum and the electron spin dipolar-nuclear spin angular momentum. This analysis yields a direct measure of the effect of the solvent system on the environment of the transition metal ion. The results are analysed in terms of the crystal field environment of the transition metal ion with contributions from (a) the dithiocarbamate ligand (b) the solvent molecules and (c) the interaction of the effective dipole moment of the polar solvent molecule with the transition metal ion complex.

Purification and Structure Determination of the GTase Inhibitor from Cacao Bean Husk Extract (Cacao Bean Husk 추출물로부터 Glucosyltransferase 저해 활성 물질의 분리 및 구조 동정)

  • 권익부;안봉전이신영
    • KSBB Journal
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    • v.11 no.5
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    • pp.536-542
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    • 1996
  • The isolation of active compounds showing the inhibitory effect on glucosyltransferase(GTase) from cacao bean husk(CBH) extract was carried out for screening of anti-plaque agents. These active compounds were purified by additional column chromatography of MCI-gel CHP-20 and Sephadex LH-20 and their chemical structures were determined by NMR and mass spectroscopy. Two compounds showing the inhibitory effect on GTase from CBH extract were obtained. These compounds showed positive reactions with anisaldehyde-H2SO4 solution and FeCl3, and were identified as dimeric flavan-3-ols on TLC. By NMR and MS data analyses, the structures of two different flavan-3-ols were identified as procyanidin B-1 and procyanidin B-3, respectively.

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