• Title/Summary/Keyword: $^1H$-nmr spectrum

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Flavone Glycosides from the Aerial Parts of Lespedeza cuneata G. Don (비수리 지상부로부터 분리한 Flavone glycosides)

  • Kwon, Dong-Joo;Kim, Jin-Kyu;Ham, Yeon-Ho;Bae, Young-Soo
    • Applied Biological Chemistry
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    • v.50 no.4
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    • pp.344-347
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    • 2007
  • The aerial parts of Lespedeza cuneata were collected, air-dried and extracted with 95% aqueous EtOH. Then it was successively partitioned with n-hexane, $CH_2Cl_2$, EtOAc and $H_2O$. Repeated Sephadex LH-20 column chromatography on the EtOAc- and $H_2O-soluble$ fractions gave four compounds. Their structures were elucidated as quercetin (1), kaempferol (2), desmodin (3) and homoadonivernith (4) on the basis of spectroscopic evidences such as $^{1}H-NMR$, $^{13}C-NMR$, 2D-NMR and MS spectrum. Desmodin (3) and homoadonivernith (4) have not been reported from this plant so far.

¹H NMR Study of Pyridine-Type Ligands Coordinated to the Paramagnetic $[Ni_3(PW_9O_{34})_2]^{12-}$ Anion

  • 우한영;김지영;소현수
    • Bulletin of the Korean Chemical Society
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    • v.16 no.12
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    • pp.1176-1179
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    • 1995
  • 1H NMR spectra of pyridine, α-, β-, and γ-picoline coordinated to the paramagnetic heteropolyanion [Ni3(PW9O34)2]12- (P2Ni3) are reported. NMR lines are assigned to [Ni3(ptl)n(PW9O34)2]12- (n=1, 2 or 3; ptl=pyridine-type ligand) on the basis of their [P2Ni3]/[ptl] dependence. The formation constants for γ-picoline complexes at 25 ℃ are K1=80, K2=610, and K3=190 L mol-1. The monopicoline complex has greater affinity for γ-picoline than P2Ni3. A degradation product, [Ni2(WO2)(PW9O34)2]12-, was also identified at low pH by measuring the NMR spectrum of pyridine coordinated to it. The isotropic NMR shifts come mainly from the contact interaction due to σ-electron delocalization.

NMR Spectroscopy and Mass Spectrometry of Benzyl Alcohol Galactoside synthesized using β-Galactosidase (베타-갈락토시데이즈를 이용하여 합성된 Benzyl Alcohol Galactoside의 NMR Spectroscopy 및 Mass spectrometry)

  • Lee, Hyang-Yeol;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.36 no.1
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    • pp.84-89
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    • 2019
  • To characterize the molecular structure of BzO-gal synthesized using Escherichia coli ${\beta}$-gal, NMR ($^1H$- and $^{13}C$-) spectroscopy and mass spectrometry of BzO-gal were conducted. $^1H$ NMR spectrum of BzO-gal showed multiple peaks corresponding to the galactosyl group, which is an evidence of galactosylation on BzOH. Five proton peaks around the aromatic region at ${\delta}_H$ 7.43 ~ 7.24 ppm and 2 peaks from ${\delta}_H$ 4.93 and 4.67 ppm were evidence of the presence of the benzyl group. Seven proton peaks at ${\delta}_H$ 4.32 ~ 3.46 ppm showed the presence of a monosaccharide and were indicative of galactosylation on BzOH. $^{13}C$ NMR spectrum also revealed the presence of 11 carbons suggestive of BzO-gal. The mass value (sodium adduct ion of BzO-gal, m/z = 293.0994) from mass spectrometry analysis of BzO-gal, and $^1H$ and $^{13}C$ NMR spectral data were in good agreement with the expecting structure of BzO-gal. We are expecting that through future study it will eventually be able to develop a new additive of low cytotoxicity.

($^{11}$B NMR study of vortex dynamics in LuNi$_2$B$_2$C

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Cho, B.K.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.107-110
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    • 2000
  • ($^{11}$B NMR measurements have been performed on single crystals of LuNi$_2$B$_2$C superconductor to investigate vortex lattice structures and dynamical behavior. The spectrum in the superconducting state is significantly broadened by local field inhomogeneity due to the vortex lattice and the peak point of the spectrum shifts toward low magnetic field due to the imperfect field penetration. The linewidth of the spectrum reflecting local field variation is much smaller than expected for conventional vortex lattices and shows peculiar increase at low temperature. Furthermore, the transverse relaxation rate, 1/T$_2$, probing the slow motion of vortices, exhibits a single peak as temperature decreases. These prominent results highlight significant fluctuation of vortices even for this low T$_c$, and nearly isotropic 3D superconductor.

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Role of NH4 and H2O in Tutton Salt (NH4)2M(SO4)2·6H2O (M=Fe and Zn) Single Crystals Studied by 1H and 14N NMR at High Temperatures

  • Park, Sung Soo;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.2
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    • pp.67-71
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    • 2017
  • At high temperature, the roles of $NH_4$ and $H_2O$ in $(NH_4)_2Fe(SO_4)_2{\cdot}6H_2O$ and $(NH_4)_2Zn(SO_4)_2{\cdot}6H_2O$ single crystals were investigated using a pulse NMR spectrometer. Temperature was shown to have a significant influence, causing changes in the deformation of $NH_4$ and $H_2O$. From the $^1H$ NMR and $^{14}N$ NMR spectrum, the forms of environment surrounding $^{14}N$ in $NH_4$ groups is more important than the loss of $H_2O$ groups. NMR studies indicate that $NH_4{^+}$ ions in Tutton salts play an important role in the changes of the crystal structure at high temperatures.

Diastereotopic $^1H-NMR$ Spectrum of Ethyl Octahydro-2,3-dioxo-6a-hydroxy-1-benzyl-cyclopenta[b]pyrrole-3a-carboxylate (Ethyl Octahydro-2,3-dioxo-6a-hydroxy-1-benzyl-cyclopenta[b]pyrrole-3a-carboxylate의 부분입체이성질성 핵자기공명 스펙트럼)

  • 김동우;김태흥;박영규;윤경원;서원준
    • YAKHAK HOEJI
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    • v.39 no.2
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    • pp.205-209
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    • 1995
  • Methylene protons of benzyl and ethyl ester in ethyl 1-benzyl-2, 3-dioxo-cyclopenta[b]-pyrrole-3a-carboxylate (A) exhibited opposite$^{1}$H-NMR spectral patterns mutually between magnetic equivalence and nonequivalence depending on concentration and temperature. The diastereotopic spectral data of compound A were reported with brief interpretation.

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Studies on the Electrochemical Behaviors, Spectrophotometric Determination of Heavy Lanthanide Ions and Heavy Metal Chelate Complexes with Bidentate Ligands(III) -Synthesis and Characterization of the Tetrakis(5,7-dichloro-8-quinolinato)(2-mercaptopyrimidinato) molybdenum(IV) Complex- (무거운 란탄이온의 전기화학적 거동, 분광학적 정량 및 중금속 이온과 두 자리 리간드 착물에 관한 연구(제 3 보): -테트라키스(5,7-디클로로-8-퀴놀리나토)(2-메르캅토피리미디나토) 몰리브데늄(IV) 착물의 합성 및 특성-)

  • Chang, Choo Hwan;Choi, Won Jong;Park, Keun Su;Son, Pyung Su;Suh, Moo Yul
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.417-424
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    • 1993
  • Eight-coordinate tetrakis molybdenum(IV) complexes containing 5,7-dichloro-8-hydroxyquinolinol(Hdcq) and 2-mercaptopyrimidine(Hmpd) has been prepared. $Mo(mpd)_4$, $Mo(dcq)(mpd)_3$, $Mo(dcq)_2(mpd)_2$, $Mo(dcq)_3(mpd)$ and $Mo(dcq)_4$ complexes have been isolated by thin-layer chromatography on silicagel plates. These complexes have been charaterized by $^1H-nmr$ spectrum and UV-Vis. spectrum. The chemical shift values of the protons ${\alpha}$ to the nitrogen in the ligands are shifted to down field. The relative intensities of the peaks which are positioned at the same proton of $Mo(dcq)(mpd)_3$ and $Mo(dcq)_3(mpd)$ are observed in 2:1 ratio, in case of $Mo(dcq)_2(mpd)_2$ appears in approximately a 1:1 ratio. The stereochemistry of the complexes in discussed in terms of their nmr spectrum and Orgel's rule. By vertue of the intensities (${\varepsilon}$>10,000~25,000) the low energy($16,600{\sim}19,800cm^{-1}$) bands are observed for the electronic spectra of the complexes are assigned as charge transfer bands.

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Characteristics of Antitumor Antibiotics HS-1 from a Stveptomyces JIoridiae SHS-1372 (Streptomyces floridae SHS-1372가 생산하는 항암항생물질 HS-1의 특성)

  • 하상철;홍순덕
    • Microbiology and Biotechnology Letters
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    • v.22 no.2
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    • pp.169-174
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    • 1994
  • Antitumor antibiotic HS-1 was purified from the culture broth of a streptomyces floridae SHS-1372 which had been isolated from soil, by solvent extraction, silica gel column chromatography and gel filtration. It was confirmed that HS-1 was active against gram positive bacteria and cancer cells(K562, P388, MCF-7, HT-29). Through the analysis of UV spectrum, melting point, IR spectrum, FAB-MS, $_{1}$H-NMR, $_{13}$C-NMR, 2D-NMR spectra, HS-1 could be identified sa the actinomycin X$_{2}$ antibiotics containing actinocine chromophore and peptides consisted of threonine, proline, methylvaline, sarcosine, D-valine and 4-ketoproline.

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Characterization of Squalene Synthase Inhibitor Isolated from Curcuma longa (울금(Curcuma longa)으로부터 분리한 squalene synthase 저해물질의 특성)

  • Choi, Sung-Won;Yang, Jae-Sung;Lee, Han-Seung;Kim, Dong-Seob;Bai, Dong-Hoon;Yu, Ju-Hyun
    • Korean Journal of Food Science and Technology
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    • v.35 no.2
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    • pp.297-301
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    • 2003
  • An inhibitor of squalene synthase, a key enzyme in the cholesterol biosynthetic pathways and a target for improved agents to lower plasma levels of low-density lipoprotein, was sequentially purified from Curcuma longa by acetone extraction, silica gel column chromatography, and sephadex LH-20 column chromatography. Active compound, YUF-01, was successfully purified and analyzed as $C_{20}H_{21}O_6$ by electron ionization mass spectrum. Through $^1H-NMR$ and $^{13}C-NMR$ analyses, YUF-01 was identified as curcumin, which showed strong inhibition of squalene synthase.

Isolation and Structure Elucidation of Acyl CoA Synthetase Inhibitor from Bacilus sp. B-6 (Bacillus sp. B-6가 생산하는 acyl CoA 합성 효소 억제 물질의 분리 및 구조 결정)

  • Kim, Kyoung-Ja;Kim, Tae-Kyong
    • YAKHAK HOEJI
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    • v.42 no.6
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    • pp.552-557
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    • 1998
  • Acyl CoA synthetase inhibitor, was purified from the culture broth of a Bacillus sp. B-6, which had been isolated from soil, by chloroform extract, silica gel column chro matography and preparative TLC. The purified acyl CoA synthetase inhibitor showed higher Antifungal activity against C. al-bicans (MIC: 8${\mu}$g/ml). Though the analysis of UV spectrum, melting point, IR spectrum, Mass-spectrum, $^1H$-NMR and $^{13}C$-NMR spectrum, the inhibitor could be identified as phenazine-l-carboxylic acid.

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