• Title/Summary/Keyword: $^2H$ NMR

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Pulsed NMR Study of $CuF_{2}.2H_{2}O$ ($CuF_{2}.2H_{2}O$의 펄스 핵자기공명 연구)

  • Lee, C.E.;Yoon, E.H.;Lee, C.H.;Kim, K.;Jeon, S.J.
    • Journal of the Korean Magnetics Society
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    • v.3 no.1
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    • pp.13-17
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    • 1993
  • We have studied $CuF_{2}.2H_{2}O$ using $^{1}H$ and $^{19}F$ pulsed nuclear magnetic resonance at 30 MHz. From the data of lineshapes, the spin-lattice relaxation times ($T_1$) and the spin echo decay times, lattice dynamics in the structure is investigated. $T_1$ data from both $^{1}H$ and $^{19}F$ NMR indicate that spin-lattice relaxation is dominated by the paramagnetic ion centers at the Cu sites. The lineshapes at room temperature appear to be strongly affected by exchange narrowing and motional narrowing.

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Molybdenum(Ⅴ)-Oxo Complexes with Oxygen, Nitrogen and Sulfur Donors. Synthesis, Spectral and Electrochemical Properties (산소, 질소, 그리고 황 주개 원자의 몰리브덴(Ⅴ)-산소 착물 합성과 분광학적 및 전기화학적 성질)

  • Kim, Hee-Jung;Koo, Bon-Kweon
    • Journal of the Korean Chemical Society
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    • v.39 no.6
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    • pp.434-439
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    • 1995
  • Six-coordinate molybdenum(Ⅴ)-oxo complexes, (R4N)[MoO(NCS)2L](R=CH3, C2H5, n-C4, H9) with S-methyl-3-(2-hydroxy-x-phenyl)methylenedithiocarbazate(L1: x=5-H) and its derivatives (L2:x=5-CH3, L3: x=3-CH3O, L4: x=5,6-C4H4 and L5: x=5-NO2) have been synthesized and the structural, spectral and electrochemical properties of the complexes have been characterized by elemental analysis, molar conductivity, UV-Vis, IR, 1H NMR, and CV (cyclic voltammetry).

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Synthesis and Characterization of Novel Oxadiazole Derivatives from Benzimidazole

  • Vishwanathan, Balasubramanaya;Gurupadayya, Bannimath
    • Journal of the Korean Chemical Society
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    • v.58 no.5
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    • pp.450-455
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    • 2014
  • In the present study, a series of novel N-(1H-benzo[d]imidazol-2-yl)methyl-5-[(hetero)aryl-1,3,4-oxadiazol-2-yl]methanamine (4a-4j) were efficiently synthesized. Condensation of hydrazide derivative 3 with various carboxylic acid derivatives yielded N-[(1H-benzo[d]imidazol-2-yl)methy](5-substituted-1,3,4-oxadiazol-2-yl)methanamine (4a-4j) and compound 5-{[(1H-benzo[d]imidazol-2-yl)methylamino]methyl}-1,3,4-oxadiazole-2-thiol (4k) was obtained on treating hydrazide 3 with carbon disulfide. All the newly synthesized analogues were characterized by IR, $^1H$ NMR, $^{13}C$ NMR and mass spectral data.

Preparation and Structure of $Re(≡NC_6H_5)(DPPE)CI_3$, $[DPPE=Ph_2PCH_2CH_2PPh_2]$ ($Re(≡NC_6H_5)(DPPE)CI_3$화합물의 합성 및 구조)

  • 박병규;정건수
    • Korean Journal of Crystallography
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    • v.6 no.2
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    • pp.93-97
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    • 1995
  • Re(≡NC6H5)(PPh3)2CI3, I, reacted with, 1,2-bis(diphenylphosphino)ethane (DPPE) to give fac-Re(≡NC6H5)(DPPE)CI3, II. The product has been characterized by 1H-NMR, elemental analysis, and X-ray crystallography. II Crystalizes in the monoclinic space group Pc, with cell parameters a=11.083(3)Å, b=10.930(1)Å, c=14.081(2)Å, β=108.37(2)°, Z=2. Least-squares refinement of the structure led to a R(wR2)factor of 0.0254(0.0607) for 2888 unique reflections of I>2σ(I) and for 352 variables.

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Vinyl Addition Copolymerization of Norbornene/5-Vinyl-2-norbornene with Cationic $\eta^{3_}$-Allyl Palladium Catalyst and Their Post-Reaction (양이온성 $\eta^{3_}$알릴 팔라듐 촉매를 사용한 노보넨/5-비닐-2-노보넨의 비닐 부가 공중합과 이를 이용한 고분자 후반응)

  • 안재철;박수현;이광희;박기홍
    • Polymer(Korea)
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    • v.27 no.5
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    • pp.429-435
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    • 2003
  • Vinyl addition copolymerizations of norbornene (NB) and 5-vinyl-2-norbomene (VNB) were carried out using a cationic η$^3$-allyl palladium catalyst in the various mole ratio of comonomers. The copolymers could be obtained in good yield (65∼85%) with high weight-average molecular weights (M$_{w}$ > 760,000). Depending on increasing VNB contents, the molecular weight and yield of the copolymers decreased. FT-IR analysis confirmed that actual contents of VNB in polymer were proportional to the feeding content of VNB. From $^1$H-NMR spectroscopy, we found that both exo and endo VNB isomer were copolymerized with NB. Thermal stabilities of NB-VNB copolymers were independent on the VNB content and their initial decomposition temperatures were about 300 C. The NB-VNB copolymers were followed by epoxidation by using m-CPBA and hydroxylation by 9-BBN, respectively, and these post-polymers were characterized by FT-IR spectroscopy and $^1$H-NMR analysis..

Synthesis and radiolabeling of PEGylated dendrimer-G2-Gemifloxacin with 99mTc to Biodistribution study in rabbit

  • Mohtavinejad, Naser;Dolatshahi, Shaya;Amanlou, Massoud;Ardestani, Mehdi Shafiee;Asadi, Mehdi;Pormohammad, Ali
    • Advances in nano research
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    • v.10 no.5
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    • pp.461-470
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    • 2021
  • Infection is one of the major mortality causes throughout the globe. Nuclear medicine plays an important role in diagnosis of deep infections such as osteomyelitis, arthritis infection, heart valve and heart prosthesis infections. Techniques such as labeled leukocytes are sensitive and selective for tracking the inflammations but they are not suitable for differentiating infection from inflammation. Anionic linear-globular dendrimer-G2 was synthesized then conjugation to gemifloxacin antibiotic. The structures were identified by FT-IR, 1H-NMR, C-NMR, LC-MS and DLS. The toxicity of gemifloxacin and dendrimer-gemifloxacin complex was compared by MTT test. Dendrimer-G2-gemifloxacin was labeled by Technetium-99m and its in-vitro stability and radiochemical purity were investigated. In-vivo biodistribution and SPECT imaging were studied in a rabbit model. Identify and verify the structure of the each object was confirmed by FT-IR, 1H-NMR, C-NMR and LC-MS, also, the size and charge of this compound were 128 nm and -3/68 mv respectively. MTT test showed less toxicity of the dendrimer-G2-gemifloxacin than free gemifluxacin (P < 0.001). Radiochemical yield was > %98. Human serum stability was 84% up to 24 h. Biodistribution study at 50 min, 24 and 48 h showed that the complex is significantly absorbed by the intestine and accumulation in the lungs and affects them, finally excreted through the kidneys, biodistribution results are consistent with results from full image means of SPECT/CT technique.

Quantitative analysis of 5-HMF produced from fructose (과당에서 전환된 5-HMF(5-hydroxymethylfurfural)의 정량적 분석)

  • Sim, Jaehoon;Shin, Soo-Jeong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.45 no.1
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    • pp.27-34
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    • 2013
  • Quantitative analysis of 5-hydroxymethylfufural (5-HMF) conversion from fructose by dehydration and rearrangement was investigated by $^1H$-NMR spectroscopic method. Fructose was converted to 5-HMF in dimethylsulfoxide (DMSO)-$d^6$ or acidic deuterium hydroxide at controlled reaction temperature and time. With addition of internal standards (biphenyl for DMSO-$d^6$ solvent, and 2,5-dihydroxybenzoic acid for deuterium oxide solvent), conversion from fructose to 5-HMF was analyzed by $^1H$-NMR spectroscopy. Quantitative analysis was run by comparison with peak area integration between of 5-HMF and internal standard. In DMSO solvent, 5-HMF was stable end product but part of 5-HMF was converted to formic and levulinic acid at acidic aqueous medium.

Characterization of pH-dependent structural properties of hydrolase PncA using NMR

  • Yi, Jong-Jae;Kim, Won-Je;Rhee, Jin-Kyu;Lim, Jongsoo;Lee, Bong-Jin;Son, Woo Sung
    • Journal of the Korean Magnetic Resonance Society
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    • v.22 no.4
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    • pp.144-148
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    • 2018
  • Catalytic enzyme Pyrazinamidase (PncA) from Mycobacterium tuberculosis can hydrolyze substrate pyrazinamide (PZA) to pyrazoic acid (POA) as active form of compound. Using NMR spectroscopy, pH-dependent catalytic properties were monitored including metal binding mode during converting PZA to POA. There seems to be a conformational change through zinc binding in active site from the perturbation of peak intensities in series of 2D HSQC spectra the conformation changes through zinc binding.

Purification and Characterization of an Antifungal Antibiotic from Bacillus subtilis LAM 97-44 (Bacillus subtilis LAM 97-44가 생산하는 항진균성 항생물질의 정제 및 특성)

  • Lee, No-Woon;Kwon, Tae-Jong;Yi, Dong-Heui
    • Applied Biological Chemistry
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    • v.46 no.2
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    • pp.69-73
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    • 2003
  • A novel antifungal antibiotic for azole-resistant Candida albicans was purified from the culture broth of Bacillus subtilis LAM 97-44 by butanol extraction, Diaion HP-20 and Dowex-50 adsorption chromatography, silica gel flash chromatography followed by HPLC and designated LAM-44A. LAM-44A was stable for 60 min at $100^{\circ}C$, and pH range from 2 to 10. MIC values were observed at $0.5-3.5\;{\mu}g/ml$ against various Candida albicans strains. The antibiotic showed no cytotoxicity for S180, MKN-45, P388, HeLa and 373 at the concentration of 1 mg/ml. LAM-f4A was colorless powder soluble in water, methanol, ethanol, butanol and negative to ninhydrin reaction. The antibiotic had maximum absorption at 273 nm in methanol, and melting point was $202^{\circ}C$. The molecular weight and formula were determined to be 282 and $C_{14}H_{34}O_5$ by $^1H-NMR,\;^{13}C-NMR$, IR spectrum and elemental analysis.

NMR Signal Assignments of Human Adenylate Kinase 1 (hAK1) and its R138A Mutant (hAK1R138A)

  • Kim, Gilhoon;Chang, Hwanbong;Won, Hoshik
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.2
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    • pp.56-60
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    • 2016
  • Adenylate kinase (AK) enzyme which acts as the catalyst of reversible high energy phosphorylation reaction between ATP and AMP which associate with energetic metabolism and nucleic acid synthesis and signal transmission. This enzyme has three distinct domains: Core, AMP binding domain (AMPbd) and Lid domain (LID). The primary role of AMPbd and LID is associated with conformational changes due to flexibility of two domains. Three dimensional structure of human AK1 has not been confirmed and various mutation experiments have been done to determine the active sites. In this study, AK1R138A which is changed arginine[138] of LID domain with alanine[138] was made and conducted with NMR experiments, backbone dynamics analysis and mo-lecular docking dynamic simulation to find the cause of structural change and substrate binding site. Synthetic human muscle type adenylate kinase 1 (hAK1) and its mutant (AK1R138A) were re-combinded with E. coli and expressed in M9 cell. Expressed proteins were purified and finally gained at 0.520 mM hAK1 and 0.252 mM AK1R138A. Multinuclear multidimensional NMR experiments including HNCA, HN(CO)CA, were conducted for amino acid sequence analysis and signal assignments of $^1H-^{15}N$ HSQC spectrum. Our chemical shift perturbation data is shown LID domain residues and around alanine[138] and per-turbation value(0.22ppm) of valine[179] is consid-ered as inter-communication effect with LID domain and the structural change between hAK1 and AK1R138A.