• Title/Summary/Keyword: $^{13}C$ NMR spectrum

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Structural Analysis of Major Antimicrobial Substance Obtained from Leaf Mustard(Brassica juncea) (갓(Brassica juncea)의 주 항균물질의 구조 분석)

  • 강성구
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.24 no.5
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    • pp.702-706
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    • 1995
  • A major component(compound A) in the ethylacetate fraction exhibited a strong antimicrobial activity was identified by UV, IR, FABMS and NMR. The compound A showed strong absorbance at 209, 259 and 359nm, indicating a flavonoid ring structure. IR spectrum possessed absorbance of OH at 3400∼3300cm-1, ketone at around 1650cm-1, and aromatic C=C at around 1660cm-1. Molecular weight of the compound A calculated as 478 from the information of m/z 479(M+H)+ and m/z 477(M-H)+ in the FABMS spectrum. Molecular formula of this compound was found to be C22H22O12 from m/z 479.1220(+3.1mmu for C22H23O12) of HRFABMS spectrum and from 13C-NMR spectrum. 1H-NMR and 13C-NMR spectra of the compound A revealed aromatic proton and benzene rings. Distortionless enhancement by polarization transfer(DEPT) exhibited that the compound A possessed 10 quaternary carbons and 3 substituted benzene rings including a methoxy group substitution. The compound A was identified as isorhamnetin 3-O-β-glucopyranoside by spectrophotometric methods in conjunction with 1H-1H COSY, 1H-13C COSY and HMBC, which revealed a flavone with OH group at 3, 5, 7, and 4' and methoxy group at 3' positions esterified to glucose.

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One-pot Synthesis of 5,7-Diaryl-3,4,6-trihydronaphthalen-2-ones (5,7-Diaryl-3,4,6-trihydronaphthalen-2-ones의 One-pot 합성)

  • Gopalakrishnan, M.;Manikandan, H.;Sureshkumar, P.;Thanusu, J.;Kanagarajan, V.
    • Journal of the Korean Chemical Society
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    • v.51 no.4
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    • pp.356-360
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    • 2007
  • 5,7-Diaryl-3,4,6-trihydronaphthalen-2-ones have been synthesized from 3,5-diaryl-cyclohex-2-en-1- ones and methyl vinyl ketone in the presence of sodium ethoxide. The products were characterized by IR, UV-Visible, 1H-NMR, 13C-NMR and mass spectral techniques. To confirm 1H and 13C signals, HSQC spectrum was recorded and analyzed.

$^{13}C$ Nuclear Magnetic Resonance Study of Graphite Intercalated Superconductor $CaC_6$ Crystals in the Normal State ($CaC_6$ 결정에 대한 정상상태에서의 $^{13}C$ 핵자기공명 측정)

  • Kim, Sung-Hoon;Kang, Ki-Hyeok;Mean, B.J.;Ndiaye, B.;Lee, Moo-Hee;Kim, Jun-Sung
    • Progress in Superconductivity
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    • v.12 no.1
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    • pp.51-56
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    • 2010
  • $^{13}C$ NMR (nuclear magnetic resonance) measurements have been performed to investigate the local electronic structure of a superconducting graphite intercalation compound $CaC_6$ ($T_c$ = 11.4 K). A large number of single crystals were stacked and sealed in a quartz tube for naturally abundant $^{13}C$ NMR. The spectrum, Knight shift, linewidth, and spin-lattice relaxation time $T_1$ were measured in the normal state as a function of temperature down to 80 K at 8.0 T perpendicular to the c-axis. The $^{13}C$ NMR spectrum shows a single narrow peak with a very small Knight shift. The Knight shift and the linewidth of the $^{13}C$ NMR are temperature-independent around, respectively, +0.012% and 1.2 kHz. The spin-lattice relaxation rate, $1/T_1$, is proportional to temperature confirming a Korringa behavior as for non-magnetic metals. The Korringa product is measured to be $T_1T\;=\;210\;s{\cdot}K$. From this value, the Korringa ratio is deduced to be $\xi$ = 0.73, close to unity, which suggests that the independent-electron description works well for $CaC_6$, without complications arising from correlation and many-body effects.

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.

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

  • 신동수;김흥재;조수동;권기락;안철진;주우홍;강진호;문병호
    • Journal of Life Science
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    • v.9 no.2
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    • pp.212-215
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    • 1999
  • Biologically active compounds in Polygonatum sibiricum were extracted using organic solvents as hexane, CHC1$_3$, n-butanol corresponding each component. Compound II was purified from hexane layer and the chemical structure of compound II was characterized using IH-nmr, 13C-nmr, DEPT135, COSY, HMQC, HMBC spectrum and MS-spectrum. Consequently, the chemical structure of compound II was determined as 2-Hydroxy-3-(9,12-(9E,12E)-Octadecadienoyloxy) propanoic acid.

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Characterization of Kraft Lignin by 13C-Nuclear Magnetic Resonance Spectroscopy (13C-NMR에 의한 크라프트 리그닌의 특성)

  • Lee, Beom-Goo;Hwang, Byung-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.17 no.4
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    • pp.44-56
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    • 1989
  • To recover much residual lignin from the black liquor of kraft pulp. the black liquor was extracted and purified with many organic solvents. Many kinds of lignins were isolated from each fraction obtained and the characteristics of these lignins investigated by $^{13}C$-NMR spectroscopy. If M$\ddot{o}$rck's method was compared with Kirk's method. M$\ddot{o}$rck's method was better than Kirk's method because the particular signals of each lignin occur more in the former than m the latter. Especially the $^{13}C$-NMR spectrum of the MCS fraction identifies with those of other researchers. The experiment that the kraft lignin from Pinus densiflora S. et Z. found in Korea was investigated by $^{13}C$-NMR spectroscopy was performed first in Korea.

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Characterization of Fibroin Biosynthesis in the 5th Instar of Bombyx mori (5령 누에에 있어서 Fibroin 생합성의 특성)

  • 이인전;여주홍
    • Journal of Sericultural and Entomological Science
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    • v.38 no.2
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    • pp.180-185
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    • 1996
  • Biosynthesis tracing of the silk fibroin in Bombyx mori silkworm was examined in vivo with isotopic [1-13C] Gly. labeling by nuclear magnetic resonance method. The [1-13C] Gly. labeled silk fibroin yielded very sharp 13C NMR signal in the posterior silk gland as well as in aqueous solution and the amound of [1-13C] Gly. labeled signal in the silkworm increased gradually and rapidly to 5-th day of fifth instar. However, the decomposition or decrease of the [1-13C] Gly. labeled signal occured from 5-th to 9-th day of fifth instar unexpectedly. These findings suggest that a relative amount of ${\alpha}$-helical portion or amorphous silk II portion was formed without any further signal from 6-th day of fifth instar to pupation. Through peak separation of orientation spectrum, between the fiber axis and the molecular bond direction, N-H bond in Bombyx mori silk fiber as well as the orientation distribution around the silk fibroin axis were determined and two kinds of peaks were also obtained from this orientation spectrum.

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