• Title/Summary/Keyword: NMR spectral analysis

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Two New Scalaranes from a Korean Marine Sponge Spongia sp.

  • Yang, Inho;Nam, Sang-Jip;Kang, Heonjoong
    • Natural Product Sciences
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    • v.21 no.4
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    • pp.289-292
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    • 2015
  • Intensive chemical investigation of Korean marine sponge Spongia sp. has led to the isolation of two new scalaranes. The planar structures of the new compounds 1 and 2 were determined through 1D and 2D NMR spectral data analysis, while the relative stereochemistry of the compounds was determined based on the analysis of $^1H-^1H$ coupling constants and NOESY spectroscopic data. Compounds 1 and 2 did not display any significant biological activities on farnesoid X-activated receptor (FXR) in co-transfection assay.

Synthesis and Antimicrobial Evaluation of Some Novel 2-(4-Chlorophenylimino) thiazolidin-4-one Derivatives

  • B'Bhatt, H.;Sharma, S.
    • Journal of the Korean Chemical Society
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    • v.56 no.3
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    • pp.341-347
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    • 2012
  • A series of 2-(4-chlorophenylimino)-5-((3-(p-substituted phenyl)-1-phenyl-1H-pyrazol-4-yl) methylene) thiazolidin-4-one ($\mathbf{3a-h}$) compounds were prepared from the 2-(4-chlorophenylimino) thiazolidin-4-one ($\mathbf{1}$) and 1-phenyl-3-(p-substituted phenyl)-1H-pyrazole-4-carbaldehyde ($\mathbf{2a-h}$). All compounds were characterized by elemental (C, H, N) analysis and spectral (FT-IR, $^1H$ NMR and GC-MS) analysis. These newly synthesized compounds were screened for their antibacterial and antifungal activities. Antimicrobial activity was observed and evaluated against the bacterial strains like Eschericha coli (MTCC 443), Pseudomonas aeruginosa (MTCC 1688), Staphylococcus aureus (MTCC 96), Streptococcus pyogenes (MTCC 442) and against the fungal strains like Candida albicans (MTCC 227), Aspergillus niger (MTCC 282) and Aspergillus clavatus (MTCC 1323). All the synthesized compounds were found to possess moderate to excellent antimicrobial activity against above selected strains.

Synthesis and Characterization of Transition Metal Complexes with Benzimidazolyl-2-hydrazones of o-anisaldehyde and Furfural

  • Mohapatra, R.K.;Mishra, U.K.;Mishra, S.K.;Mahapatra, A.;Dash, D.C.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.926-931
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    • 2011
  • A series of complexes of the type [$ML_2Cl_2$], where L=2-(o-anisylidene-2'-imino) amino benzimidazole (AIAB) and 2-(furfurylidene imino) amino benzimidazole (FIAB), M=Cu(II), Co(II), Ni(II) and Zn(II), have been synthesized and characterized on the basis of elemental analysis, thermal analysis, molar conductivity, magnetic moment, electronic, infrared, $^1H$-NMR spectral studies. The results are in consistent with bidentate chelation of ligand with azomethine nitrogen and ring nitrogen donors. All these Schiff bases and their complexes have also been screened for their antibacterial (Bacillus subtilis, Bacillus stearothermophilus, Escherichia coli and Salmonella typhi) and antifungal activities (Aspergillus niger and Aspergillus flavus).

Studies on the Chemical Constituents of Lysimachia Clethroides (큰까치수영의 구성성분)

  • 김진숙;김형자;박호군
    • YAKHAK HOEJI
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    • v.37 no.4
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    • pp.325-330
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    • 1993
  • Four flavonoide glycosides and (-)-Epicatechin were isolated from the aqueous extracts of dried whole part of Lysimachia clethroides Duby(Primulaceae). They were 3-0-Methyl-quercetin-7-0-[$\alpha$-L- rhamnopyranosyl (1-2) glucopyranoside], Quercetin-3-0-$\beta$-D-glucopyranoside, Kaempferol-3-0-$\beta$-D-glucopyranoside, Kaempferol-3-0-[$\alpha$-L-rhamnopyranosyl (1-6)-$\beta$-D-glucopyranoside] and (-)-Epicatechin. 3-0-[$\alpha$-L-rhamnopyranosyl (1-6)-$\beta$-D-glucopyranoside]and (-)-Epicatechin. 3-0-Methyl-quercetin-7-0-[$\alpha$-L-rhamnopyranosyl (1-2)-$\beta$-D-glucopyranoside] and (-)-Epicatechin were first isolated from this plant. Their structures were elucidated by spectral analysis [$^{1}$H-, $^{13}C-$ NMR, $^{1}$H-$^{1}$H-COSY, DEPT-analysis, HMQC(Heteronuclear multiple quantum coherence), FAB-MS].

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Triterpenoids from the Flower of Viburnum opulus var. clavescens for. sterile (불두화(Viburnum opulus var. clavescens for. sterile) 꽃의 트리테르페이드 성분)

  • Choi, Seong Yeon;Kim, Myong Jo;Chun, Wanjoo;Kwon, Yongsoo
    • Korean Journal of Pharmacognosy
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    • v.53 no.3
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    • pp.133-137
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    • 2022
  • Four known triterpenoids and one sterol glycoside were isolated from Viburnum opulus var. clavescens for. sterile flowers. By the spectral data analysis, we determined to be the structures of isolated compounds as 𝛼-amyrin (1), ursolic aldehyde (2), maslinic acid (3), ursolic acid (4) and 𝛽-sitosterol-3-O-glucoside (5). Among the isolated compounds, we revised 13C-NMR chemical shifts of ursolic aldehyde (2) using DEPT and HMBC spectra analysis. 𝛼-Amyrin (1), ursolic aldehyde (2), maslinic acid (3) and 𝛽-sitosterol-3-O-glucoside (5) were isolated for the first time from this plant.

A Review: Synthesis and characterization of metals complexes with paracetamol drug

  • AL-Ayash, Salam R;AL-Noor, Taghreed H
    • Analytical Science and Technology
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    • v.35 no.4
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    • pp.143-152
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    • 2022
  • In this review, previous studies on the synthesis and characterization of the metal Complexes with paracetamol by elemental analysis, thermal analysis, (IR, NMR and UV-Vis (spectroscopy and conductivity. In reviewing these studies, the authors found that paracetamol can be coordinated through the pair of electrons on the hydroxyl O-atom, carbonyl O-atom, and N-atom of the amide group. If the paracetamol was a monodentate ligand, it will be coordinated by one of the following atoms O-hydroxyl, O-carbonyl or N-amide. But if the paracetamol was bidentate, it is coordinated by atoms (O-carbonyl and N-amide), (O-hydroxyl and N-amide) or (O-carbonyl and O-hydroxyl). The authors also found that free paracetamol and its complexes have antimicrobial activity.

Confirmation of Enzymatic Synthesis of 1, 2-Octanediol Galactoside using Mass Spectrometry and NMR Spectroscopy (Mass spectrometry와 NMR Spectroscopy를 이용한 1, 2-Octanediol Galactoside의 효소합성 확인)

  • Lee, Hyang-Yeol;Jin, Hong-Jong;An, Seung Hye;Lee, Hye Won;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.38 no.3
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    • pp.824-831
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    • 2021
  • 1, 2-Octanediol galactoside (OD-gal) has been synthesized from 1, 2-octanediol (OD), as a safer cosmetic preservative, using recombinant Escherichia coli β-galactosidase (β-gal). To confirm the molecular structure of synthesized OD-gal, mass spectrometry and NMR (1H- and 13C-) spectroscopy of OD-gal were carried out. In the reaction mixture, a sodium adduct ion of OD-gal (m/z=331.1732) was identified using mass spectrometry analysis. In addition, 1H NMR spectrum of OD-gal showed multiple peaks corresponding to the galactosyl group, which is evidence of galactosylation on OD. Downfield proton peaks at δH 4.39 ppm and multiple peaks from δH 3.98~3.55 ppm were indicative of galactosylation on OD. Up field proton peaks at δH 1.52~1.26 ppm and 0.89 ppm showed the presence of CH2 and CH3 protons of OD. 13C NMR spectrum revealed the presence of 24 carbons suggestive of α- and β-anomers of OD-gal. Among 14 carbon peaks from each anomer, the 4 peaks at δC 31.4, 29.0, 22.3, and 13.7 ppm were assigned to be overlapped showing only 24 peaks out of a total of 28 peaks. The mass value from mass spectrometry analysis of OD-gal, and 1H and 13C NMR spectral data were in good agreement with the expecting structure of OD-gal. Finally, we identified a galactose molecule from the hydrolysate of OD-gal using β-gal. We are expecting that through future study it will eventually be able to develop a safe cosmetic preservative.

Spectrophotometric Analysis of Behavior to Tyrosine Residue in the Yellow Fluorescent Cocoon of Bombyx mori (황색 형광견 중 Tyrosine잔기 거동의 분광학적 분석)

  • Yeo, Ju-Hong;Lee, In-Jeon
    • Journal of Sericultural and Entomological Science
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    • v.39 no.2
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    • pp.169-173
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    • 1997
  • The behavior of tyrosine(Tyr.) residue of Bombyx mori silk fiber from yellow fluorescent cocoon has been examined for the dependence of pH in aqueous silk solution under the presence of orange II salt. Through the peak separation of angular dependence of spectral pattern of 15N-Tyr. and [1-13C]-Tyr. between the fiber axis and the molecular bond direction, N-H bond in fiber as well as the orientation distribution around the fiber axis were analyzed. Also, and sericin component was obtained from these angular dependence of oriented spectral pattern. The pH dependence of the 13C NMR chemical shift of B. mori silk fibroin was examined in aqueous solution in the presince of orange II are broad at pH$\geq$7.0. However, these become sharper at pH$\geq$8.0 and remain sharp at higher pH. In these higher pH range, a chemical shift change occurs due to the deprotonation of the Tyr. side group of fibroin. At higher pH. such a hydrophobic cluster is destroyed because of the electrostatic interaction according to the deprotonation of the Tyr-OH group.

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An NMR Study on Molecular Motions of $\alpha$,2,6-Trichlorotoluene in Solution State

  • Ahn, Sang-Doo;Lee, Jo-Woong
    • Bulletin of the Korean Chemical Society
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    • v.15 no.7
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    • pp.553-559
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    • 1994
  • Dynamics of $CH_2CI$ group in ${\alpha},2,6$-trichlorotoluene dissolved in $CDCl_3$ was studied by observing various relaxation modes for $^{13}C$ under proton undecoupled condition. Partially relaxed $^{13}C$ spectra were obtained at $34^{\circ}C$ as a function of evolution time after applying various designed pulse sequences to this $AX_2$ spin system. It was found that nonlinear regression analysis of the relaxation data for these magnetization modes could provide the information about dipolar and spin-rotational auto-correlation and cross-correlation spectral densities for fluctuation of the $^{13}C-^1H$ internuclear vector in $CH_2Cl$ group. The results show that the effect of cross-correlation is comparable in magnitude to that of auto-correlation and the relaxation in this spin system is dominated by dipolar mechanism rather than spin-rotational one. From the resulting spectral density data we could calculate the bond angle ${\angle}HCH\;(105.1$^{\circ}$) and elements of the rotational diffusion tensor for $CH_2Cl$ group.

Investigation of $xV_2O_5-B_2O_3$ and $xV_2O_5-B_2O_3-yNa_3O$ Glasses by $^{11}B MAS$ NMR

  • Kim, Sun-ha;Han, Oc-Hee;Kang, Jae-Pil
    • Journal of the Korean Magnetic Resonance Society
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    • v.9 no.1
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    • pp.61-66
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    • 2005
  • $^{11}B MAS NMR$ spectra of binary glass system $xV_2O5-B_2O_3$ and ternary glass system $xV_2O5-B_2O_3-yNa_2O$ (x = $V_2O_5 mol%/$B_2O_3$ mol%, y = $Na_2O$ mol$/$B_2O_3$ mol%) were acquired. $BO_3$ units are dominant components in the spectra of $xV_2O_5-B_2O_3$glass systems while both $BO_3$ and $BO_4$ unit appear in comparable amounts in the spectra of $xV_2O_5-B_2O_3-yNa_2O$ glass systems. More $BO_3$ units were monitored for higher $V_2O_5$ contents while more $BO_4$ unit for higher $Na_2O$ contents. Quadrupole parameters such as $e^2qQ$ and $\eta$ obtained form spectral simulation indicate that $e^2qQ$ has a maximum value at x = y 1 and $\eta$ decreases and increases as x or y grows, respectively. Our results suggest that $V_2O_5$ and $Na_2O$ play opposite roles in the ternary glasses.

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