• Title/Summary/Keyword: 탄소-13 NMR

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Sonochemical Synthesis of Closed [5,6]-bridged Aziridino[70]fullerene Derivative and Self-assembled Multilayer Films

  • Yoon, Shin-Sook;Hwang, Sung-Ho;Hong, Sung-Kyu;Lee, Jeong-Ho;Ko, Weon-Bae
    • Carbon letters
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    • v.10 no.4
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    • pp.325-328
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    • 2009
  • This cycloaddition of [70]fullerene with methyl azidoacetate in benzene under ultrasonic irradiated condition afforded the closed [5,6]-bridged aziridino[70]fullerene derivative, which was unusual product of cycloaddition to the 5,6-junction of fullerene. Its structure was determined by FAB-MS, UV-vis, $^1H-$ and $^{13}C$-NMR spectral data. The closed [5,6]-bridged aziridino[70]fullerene-functionalized gold nanoparticle films were self-assembled using the layer-by-layer method on the reactive of glass slides functionalized with 3-mercaptopropyl trimethoxysilane. The functionalized glass slides were alternately soaked in the solution containing closed the [5,6]-bridged aziridino[70]fullerene and 4-aminothiophenoxide/hexanethiolate-protected gold nanoparticles. The closed [5,6]-bridged aziridino[70]fullerene-functionalized gold nanoparticle films have grown up to 5 layers depending on the immersion time. The self-assembled nanoparticle multilayer films were characterized using UV-vis spectroscopy showed that the surface plasmon band of gold at 527 nm gradually became more evident as successive layers were added to the films.

Molecular Structure of PCP Pincer Complexes: Poisoning Catalyst on the Dehydrogenation of Alkanes (알칸의 탈수소화반응에서의 촉매독 화합물의 분자구조)

  • Lee Ji Hyun;Chun Sang Jin;Kwon Ki Hyeok;Lee Do Weon
    • Korean Journal of Crystallography
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    • v.16 no.1
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    • pp.43-53
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    • 2005
  • The dihydrido P-C-P pincer complex, $IrH_2{C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (1), was successfully prepared from the reaction of the hydrochloride complex, $IrClH (C_6H_3-2,6-(CH_2PBu_2^t)_2}$, and super acid $(LiBEt_3H)$ under 1 atm of hydrogen in pentane solution at room temperature and followed by Heating at $130^{\circ}C$ in vacuo. Jensen recently found that the dihydrido P-C-P pincer complex 1 is a highly active homogeneous catalyst for the transfer dehydrogenation of alkanes with unusual longterm stability at temperatures as high as $200^{\circ}C$. The treatment of dihydrido complex 1 with nitrogen, water, carbon dioxide, and carbon monoxide in presence of tert-butylethylene (the) at room temperature in an appropriate solution gave the dinitrogen complex, $[Ir{C-6H_3-2,6-(CH_2PBu_2^t)_2}]_2({\mu}-N_2)$ (2), the hydrido hydroxyl complex, $IrH(OH){C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (3), the carbon dioxide complex, $Ir({\eta}^2-CO_2) {C_6H_3-2,6-(CH_2PBu_2^t)_2}$ (including the bicarbonate complex, $IrH({\kappa}^2-O_2COH){C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(4))$, and the carbonyl complex, $Ir(CO) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(5)$ (including the carboxyl complex, $IrH(C(O)OH) {C_6H_3-2,6-(CH_2PBu_2^t)_2}\;(6))$, in good yield, respectively. These P-C-P iridium complexes were isolated and characterized by $^1H,\;^{13}C,\;^{31}P\; NMR$, and IR spectroscopy. In addition, the complexes (1-6) were characterized by a single crystal X-ray crystallography. These complexes account for these small molecules' inhibition of dehydrogenation of alkanes catalyzed by the dihydrido complex 1.

Analysis of ${\beta}-(1{\to}3)(1{\to}6)-Glucan$ Produced by Aureobasidium pullulans IMS-822 (Aureobasidium pullulans IMS-822가 생산하는 ${\beta}-(1{\to}3)(1{\to}6)-Glucan$의 특성 분석)

  • Lee, Seog-June;Ahn, Keug-Hyun;Park, Chan-Sun;Yoon, Byung-Dae;Kim, Min-Soo
    • Korean Journal of Microbiology
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    • v.45 no.1
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    • pp.63-68
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    • 2009
  • The exo-polysaccharide producing microorganism, Aureobasidium pullulans IMS-822, was isolated and identified from soil. The viscosity-average molecular weight of exo-polysaccharide was calculated as $8.9{\times}10^5$ by Mark-Houwink equation. The sugar component of exo-polysaccharide was determined as glucose by HPLC analysis. The IR spectra indicated that the exo-polysaccharide has an absorption peak at 890 $cm^{-1}$ for the ${\beta}-configuration$ of D-glucan. The $^{13}C$ NMR signal at ${\delta}$ 86.62 ppm arose from the substituted C-3 of glucose. The signal at ${\delta}$ 72.11 ppm was assigned to C-6 of branched ${\beta}-(1{\to}3)-D-glucosyl$ residues. Viscosity and Congo red reaction indicated that {\beta}-(1{\to}3)(1{\to}6)-glucan$ produced by A. pullulans IMS-822 has a highly ordered hydrogen-bond dependent conformation in aqueous solution, which collapses in strong alkaline solution.

Solvent-Polymer Interactions for Stable Non-Aqueous Graphene Dispersions in the Presence of PVK-b-PVP Block Copolymer (PVK-b-PVP 블록 공중합체의 존재 하에서 안정한 비 수계 그래핀 분산액을 위한 용매-고분자 상호작용에 관한 연구)

  • Park, Kyung Tae;Perumal, Suguna;Lee, Hyang Moo;Kim, Young Hyun;Cheong, In Woo
    • Journal of Adhesion and Interface
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    • v.18 no.3
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    • pp.109-117
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    • 2017
  • Poly(N-vinyl carbazole) (PVK) homopolymer, poly(4-vinylpyridine) (PVP) homopolymer, and PVK-b-PVP block copolymer were synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization and the polymers were used to prepare non-aqueous graphene dispersions with four different solvents, ethanol, N-methyl-2-pyrrolidone (NMP), dichloromethane (DCM), and tetrahydrofuran (THF). $^1H-$ and $^{13}C-NMR$ spectroscopy, size exclusion chromatography (SEC), and differential scanning calorimetry (DSC) were carried out to confirm the chemical structure of the polymers. Stability of graphene dispersions was measured by on-line turbidity measurement. Time-dependent Turbiscan Stability Index (TSI) values were interpreted in terms of surface tension (${\sigma}$) and solubility parameter (${\delta}$) among solvents, polymers, and graphene. It was confirmed that the solubilities of polymer and surface tension between solvent and graphene affected the dispersion stability of graphene. PVK-b-PVP block copolymer could effectively maintain the low TSI values of graphene dispersions in ethanol and THF, which have been known as poor solvents for graphene dispersions. It can also be noted that DCM shows good dispersion stability comparable to NMP, which has been known as the best solvent for graphene dispersion.

Synthesis of Renewable Resource-derived Furan-based Epoxy Compounds and Their Adhesive Property (재생자원 유래 퓨란계 에폭시 화합물의 합성 및 접착 특성)

  • Lee, Jae-Soung;Lee, Sang-Hyeup;Jeong, Jaewon;Kim, Baekjin;Cho, Jin Ku;Kim, Hyun Joong
    • Journal of Adhesion and Interface
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    • v.11 no.2
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    • pp.41-49
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    • 2010
  • Furan-containing epoxide monomers (8, 9) were designed and synthesized as carbon-neutral, environment-friendly adhesion material. Bicyclic skeleton were constructed using the Diels-Alder reaction of furan and methyl acrylate, both readily accessible starting material from a biomass via bio-refinery process. After reduction of ester functionality, resulting hydroxyl moieties were coupled to epichlorohydrin to provide the epoxy-functionalized furanic monomers (8, 9). The structure of new furanic monomers was confirmed by $^1H$ and $^{13}C$ NMR spectroscopy. As UV-curable monomers, basic properties such as UV curing time and the extent of UV curing were evaluated by photo DSC. Photo-curing shrinkages were measured by linear variable differential transformer transducer (LVDT) and the effect of molecular structure on shrinkage was considered. In addition, new synthetic compounds showed the shear strength over 3 MPa when they were photo-cured between polycarbonate plates, which indicates these compounds are feasible to use as photo-curable adhesive materials.

Isolation and Structural Determination of Antifungal Antibiotic from Streptomyces hygroscopicus MJM1004 (Streptomyces hygroscopicus MJM1004가 생산하는 항진균성 항생 물질의 분리 및 구조 결정)

  • Bae, Ju-Yun;Kwon, Hyong-Jin;Suh, Joo-Won
    • Applied Biological Chemistry
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    • v.42 no.4
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    • pp.271-276
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    • 1999
  • Several Streptomyces strains were tested for potent antifungal agents active against phytopathogenic fungi. Among the tested, S. hygroscopicus MJM1004 showed a potent antifungal activity when assayed using Candida albicans as indicator organism. With the strain of MJM1004, fermentation medium for the production of an antifungal agent was developed with varying carbon sources, nitrogen sources, and mineral elements, which resulted in the highest productivity in the medium containing 2% soybean meal, 1% glucose, 2% starch, 0.3% $CaCO_3$, 0.05% $MgSO_4{\cdot}7H_2O$, 0.05% $K_2HPO_4$. The active compound showed a broad spectrum of antifungal activity against several plant pathogenic fungi. The antifungal compound was purified and showed the physicochemical characteristics similar to azalomycin F complex in NMR and MS analysis.

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Improving Productivity of Pravastatin, HMG-CoA Reductase Inhibitor (HMG-CoA Reductase Inhibitor인 Pravastatin의 생산성 향상)

  • Jeon, Dong-Soo;Bai, Dong-Hoon
    • Food Engineering Progress
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    • v.13 no.4
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    • pp.243-250
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    • 2009
  • Pravastatin sodium, competitive inhibitors of HMG-CoA(3-hydroxy-3-methylglutaryl coenzyme A) reductase, is produced from the culture broth of Streptomyces carbophilus KCCM 10370, The production of Pravastatin sodium was increased about 45 fold compared to wild type by UV mutation. Production of Pravastatin was also improved by continuous feeding of Compactin sodium to 24% and bioconversion ratio was also increased to 4.3% by intermittent addition. In main culture, concentration of Compactin sodium was kept less than 0.1%(w/v) under continuous feeding of Compactin sodium then product was 0.49% and bioconversion was 70%. After finishing the fermentation, Pravastatin was purified by various chromatographies such as Diaion HP20 resin column, Partition, and ODS(Octa-Decylsilyl Silicagel) resin column with a final yield of 70~72% and over 99.7% purity. The IR, UV, and NMR study of the purified Pravastatin sodium showed the same pattern as that of EP(European Pharmacopoeia).

Chemical and Spectroscopic Characterization of Peat Moss and Its Different Humic Fractions (Humin, Humic Acid and Fulvic Acid) (피트모스에서 추출한 휴믹물질(휴믹산, 풀빅산, 휴민)의 화학적 및 분광학적 물질특성 규명)

  • Lee Chang-Hoon;Shin Hyun-Sang;Kang Ki-Hoon
    • Journal of Soil and Groundwater Environment
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    • v.9 no.4
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    • pp.42-51
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    • 2004
  • Peat humin(p-Humin), humic acid(p-HA) and fulvic acid(p-FA) were isolated from Canadian Sphagnum peat moss by dissolution in 0.1M NaOH followed by acid precipitation. After purification cycles, they are characterized for their elemental compositions and, acid/base properties. Functionalities and carbon structures of the humic fractions were also characterized using FT-IR and solid state $^{13}C$-NMR spectroscopy. Those results are compared with one another and with soil humic substances from literatures. Main purpose of this study was to present a chemical and spectroscopic characterization data of humic substance from peat moss needed to evaluate its environmental applicability. The relative proportions of the p-Humin, p-HA and p-FA in the peat moss was $76\%,\;18\%,\;and\;3\%$, respectively, based on the total organic matter content ($957{\pm}32\;g/kg$). Elemental composition of p-Humin were found to be $C_{1.00}H_{1.52}O_{0.79}N_{0.01}$ and had higher H/C and (N+O)/C ratio compared to those of p-HA($C_{1.00}H_{1.09}O_{0.51}N_{0.02}$) and p-FA($C_{1.00}H_{1.08}O_{0.65}N_{0.01}$). Based on the analysis of pH titration data, there are two different types of acidic functional groups in the peat moss and its humic fractions and their proton exchange capacities(PEC, meq/g) were in the order p-FA(4.91) >p-HA(4.09) >p-Humin(2.38). IR spectroscopic results showed that the functionalities of the peat moss humic molecules are similar to those of soil humic substances, and carboxylic acid(-COOH) is main function group providing metal binding sites for Cd(II) sorption. Spectral features obtained from $^{13}C$-NMR indicated that peat moss humic molecules have rather lower degree of humification, and that important structural differences exist between p-Humin and soluble humic fractions(p-HA and p-FA).