• Title/Summary/Keyword: $^1H$ and $^{13}C$ NMR

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Structure Identification and Cage Occupancy Analysis of the Mixed Gas Hydrates Containing 1-Propanol and 2-Propanol (propanol계 혼합 하이드레이트의 구조 및 동공 점유 분석)

  • Lee, Youngjun;Lee, Seungmin;Park, Sungmin;Kim, Yunju;Seo, Yongwon
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.11a
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    • pp.121.1-121.1
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    • 2011
  • 일반적으로 알콜계 물질은 가스 하이드레이트 형성에 저해제로 사용된다고 알려져 있으나, 최근의 연구를 통해 2-propanol이 일부 조건에서 촉진효과가 나타난다고 보고되고 있다. 본 연구에서는 알콜계 물질인 1-propanol과 2-propanol의 가스 하이드레이트 격자내로의 포집여부와 그로 인한 촉진 혹은 저해 작용 그리고 구조적 특성에 대해 알아보았다. $CO_2$$CH_4$ 기체에 대하여 1-propanol 혹은 2-propanol을 첨가하여 형성된 혼합 하이드레이트의 3상평형 기상(V)-물(Lw)-하이드레이트(H))을 측정하였다. 그 결과 $CO_2$의 경우 1-propanol과 2-propanol이 저해 작용을 함을 확인하였으며 농도가 높을수록 저해작용이 커짐을 알 수 있었다. 반면, $CH_4$의 경우 1-propanol에서는 저해 및 촉진효과가 거의 나타나지 않았지만, 2-propanol에서는 촉진효과가 나타났으며 5.6 mol%에서 촉진효과가 가장 크게 나타났다. 혼합 하이드레이트의 구조규명 및 동공 점유 분석을 위해 $^{13}C$ NMR과 XRD분석을 하였으며, 그 결과 2-propanol과 1-propanol을 포함하는 혼합 하이드레이트는 구조 II를 형성하며, 2-propanol과 1-propanol은 큰 동공에 포집되고, 기체는 작은 동공에 포집됨을 확인할 수 있었다. 본 연구의 결과는 알콜계 물질을 첨가제로 사용하는 가스 하이드레이트 공정에서 매우 유용한 기초자료가 될 것으로 사료된다.

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Structural Characteristics of the Water Soluble Browning Reeaction Products Isolated from Korean Red Ginseng (홍삼으로부터 분리한 수용성 갈변물질의 구조 특성)

  • 이종원;고학룡;심기환
    • The Korean Journal of Food And Nutrition
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    • v.11 no.5
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    • pp.499-505
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    • 1998
  • The purpose of this study was to ivestigate the structural characteristics of waste soulble browning reaction prodcuts (WS-BRPs) isolated from Korean red ginseng. They all showed the maximum absorbances at near 280 nm. Their IR spectra suggested the presence of hydroxyl, amide carbonyl and aliphatic methine groups. From sugar analysis it was identified that L and S-1 contained two kinds of suggar, glucose and xylose, and S-2, a fructose together with glucose and xylose. Thirteen different amino acids were identified in L. Ten amino acids from S-1 and seven amino acids from S-2 were identified using Auto Amino Acid Analyzer. Glycine, serine and glutamic acid in S-1 and one unknown amino acid and glycine in S-2 were detected as the major amino acids, respectively. From the 1H-and 13C-NMR spectra, it was identified that a number of sugar moieties, carbonyl and carbon double bonds (only in S-2) were contained in the three WS-BRP components. Approximate number of sugar moiety of L, S-1 and S-2 was determined to be 8∼10, 9∼11 and 4∼5, respectively. Contents of nitrogen, carbon and hydrogen showed L>S-1>S-2.

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Synthesis and Physical Properties of Decylbithiophene End-Capped Oligomers Based on Naphthalene, Anthracene and Benzo[1,2-b:4,5-b']dithiophene

  • Jang, Sang-Hun;Tai, Truong Ba;Kim, Min-Kyu;Han, Jeong-Woo;Kim, Yun-Hi;Shin, Sung-Chul;Yoon, Yong-Jin;Kwon, Soon-Ki;Lee, Sang-Gyeong
    • Bulletin of the Korean Chemical Society
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    • v.30 no.3
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    • pp.618-622
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    • 2009
  • The new candidates for OTFTs, which were composed of naphthalene, anthracene, benzo[1,2-b:4,5-b’]dithiophene and 2-decylbithiophene end-capper were synthesized under Suzuki coupling reaction conditions. All of the oligomers were characterized by FT-IR, mass analysis, UV-vis, PL spectrum, cyclic voltametry (CV), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), $^1H-NMR\;and\;^{13}C-NMR$. Investigation of physical properties showed that all of the oligomers have higher oxidation potential and good thermal stability. Especially, DBT-DtB-DBT is soluble in common solvents and suitable for low cost processing technologies.

Synthesis, Spectroscopic Studies and Biological Applications of Organotin(IV) Derivatives of 3-[N-(4-Nitrophenyl)-amido]propenoic Acid and 3-[N-(4-Nitrophenyl)-amido]propanoic Acid

  • Shahid, Khadija;Shahzadi, Saira;Ali, Saqib;Mazhar, M.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.1
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    • pp.44-52
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    • 2006
  • New organotin(IV) derivatives with general formulae R_2SnL_2 and R_3SnL, where R = methyl, n-butyl, n-octyl and phenyl and HL is either 3-[N-(4-nitrophenyl)amido]-propenoic acid or 3-[N-(4-nitrophenyl)amido] propanoic acid have been synthesized in 1 : 2 and 1 : 1 molar ratio by different methods. The FTIR spectra clearly demonstrated that the organotin(IV) moieties react with [O,O] atoms of the ligands. The bonding and coordination behavior in these complexes are discussed on the basis of multinuclear (^1H,\,^{13}C,\,^{119}Sn) NMR and mass spectrometric studies. Antibacterial, and antifungal screening tests were performed for these compounds and reported here. These values were compared to those of the precursors and it was found that diorganotin(IV) complexes exhibit less activity as compared to triorganotin(IV) complexes . LD_{50} data were obtained by Brine Shrimp assay method. Insecticidal activity was performed for selective compounds by contact toxicity method.

Antishigellosis and Cytotoxic Potency of Crude Extracts and Isolated Constituents from Duranta repens

  • Nikkon, Farjana;Habib, M. Rowshanul;Karim, M. Rezaul;Hossain, M. Shamim;Mosaddik, M. Ashik;Haque, M. Ekramul
    • Mycobiology
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    • v.36 no.3
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    • pp.173-177
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    • 2008
  • The crude ethanol extracts (stem and fruits), their fractions and two triterpenes, $\beta$-Amyrin and 12-Oleanene 3$\beta$, 21$\beta$-diol, isolated as a mixture from the chloroform soluble fraction of an ethanolic extract of Duranta repens stem, were evaluated for antibacterial, antifungal activities by the disc diffusion method and cytotoxicity by brine shrimp lethality bioassay. The structures of the two compounds were confirmed by IR, $^1H$-NMR, $^{13}C$-NMR and LC-MS spectral data. The chloroform soluble fraction of stem and ethanol extract of fruits possess potent antishigellosis activity and also exhibited moderate activity against some pathogenic bacteria and fungi but the isolated compound 1 (mixture of $\beta$-Amyrin and 12-Oleanene 3$\beta$, 21$\beta$-diol) showed mild to moderate inhibitory activity to microbial growth. The minimum inhibitory concentrations (MICs) of the extracts (stem and fruits), their fractions and compound 1 were found to be in the range of 32$\sim$128 ${\mu}g/ml$. The chloroform soluble fractions of stem and ethanol extract of fruit showed significant cytotoxicity with $LC_{50}$ value of 0.94 ${\mu}g/ml$ and 0.49 ${\mu}g/ml$, respectively against brine shrimp larvae.

Coordination of an Amino Alcohol Schiff Base Ligand Toward Cd(II)

  • Mardani, Zahra;Hakimi, Mohammad;Moeini, Keyvan;Mohr, Fabian
    • Journal of the Korean Chemical Society
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    • v.63 no.1
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    • pp.29-36
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    • 2019
  • A potentially tetradentate Schiff base ligand, 2-((2-((pyridin-2-ylmethylene)amino)ethyl)amino)ethan-1-ol (PMAE), and its cadmium(II) complex, [$Cd(PMAE)I_2$] (1), were prepared and characterized by elemental analysis, FT-IR, Raman, $^1H$ and $^{13}C$ NMR spectroscopies and single-crystal X-ray diffraction. In the crystal structure of 1, the cadmium atom has a slightly distorted square-pyramidal geometry and a $CdN_3I_2$ environment in which the PMAE acts as an $N_3$-donor. In the crystal packing of the complex, the alcohol and amine groups of the coordinated ligands participate in hydrogen bonding with iodide ions and form $R^2{_2}(14)$ and $R^2{_2}(8)$ hydrogen bond motifs, respectively. In addition to the hydrogen bonds, the crystal network is stabilized by ${\pi}-{\pi}$ stacking interactions between pyridine rings. The thermodynamic stability of the isolated ligand and its cadmium complex along with their charge distribution patterns were studied by DFT and NBO analysis.

Synthesis of Asymmetric Pyrazoline Derivatives from Phenylthiophenechalcones; DFT Mechanistic Study

  • Aboelnaga, Asmaa;Mansour, Eman;Ahmed, Hoda. A.;Hagar, Mohamed
    • Journal of the Korean Chemical Society
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    • v.65 no.2
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    • pp.113-120
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    • 2021
  • New phenylthiophenechalcones,1-(biphenyl-4-yl)-3-(5-phenylthiophen-2-yl)prop-2-en-1-one (3a) and 3-(5-phenylthiophen-2-yl)-1-(4-(piperidin-1-yl) phenyl) prop-2-en-1-one (3b) were synthesized, next, their treatment with thiosemicarbazide in ethanol afforded their pyrazoline derivatives (4a) and (4b), respectively. The molecular structures of the synthesized compounds were confirmed via elemental analysis, FT-IR, 1H, 13C NMR and mass spectroscopy. The geometrical elucidation of four suggested conformers has been studied for these compounds. DFT calculations have been performed to study the stability and the structural parameters of the predicted conformers and revealed that orientation of the biphenyl and the phenylthiophene moieties affect the stability of the estimated conformers of the synthesized chalcones and pyrazoline. Moreover, two reaction mechanisms have been proposed to illustrate the reaction products and the DFT calculations have been used to confirm the reaction mechanism of the pyrazoline compounds.

Cytotoxicity of the Components of Albizzia julibrissin (합환피 (Albizzia julibrissin)의 성분이 종양세포에 미치는 영향)

  • Choi, Boung-Don;Ryeom, Kon
    • Biomolecules & Therapeutics
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    • v.7 no.4
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    • pp.371-376
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    • 1999
  • By cytotoxicity screening of the 65 Korean medicinal plants against leukemia L1210 and P388D$_{1}$ cell line using the MTT assay in vitro, Albizzia julibrissin was studied. This plant was extracted with MeOH and MeOH extract was solvent-fractionated with CHCl$_{3}$, EtOAc and n-BuOH in sequence. Each fraction by various solvents system was purified by column chromatography and preparative TLC, and four compounds were isolated. The structure of each compound was deduced from UV, IR, $^{1}$H-HMR, $^{13}$ C-NMR and CI-MS spectral data. The cytotoxic activity ($IC_{50}$/_ of the compounds, quercetin-3-rhamnoside, 4',5,7-trihydroxyfla-van-3-glucoside, spinasterol-3-glucoside and acacic acid lactone, were evaluated as 5 $\mu\textrm{g}$/ml, 2$\mu\textrm{g}$/ml, 1 $\mu\textrm{g}$/ml against L1210 and as 9$\mu\textrm{g}$/ml, 10$\mu\textrm{g}$/ml, 1.5 $\mu\textrm{g}$/ml, 1.5 $\mu\textrm{g}$/ml and 0.9 $\mu\textrm{g}$/ml against P388D$_{1}$, respectively.

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Modulative Effect of Human Hair Dermal Papilla Cell Apoptosis by Acertannin from the Barks and Xylems of Acer ginnala Maxim (신나무 유래 Acertannin의 인체 모유두 세포 Apoptosis 조절 효능)

  • Joung, Seo Woo;Choi, Sun Eun
    • Korean Journal of Pharmacognosy
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    • v.49 no.1
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    • pp.7-14
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    • 2018
  • We isolated gallotannin, 2,6-digalloyl-1,5-anhydroglucitol, known as acertannin (1), from the barks and xylems of Acer ginnala Maxim. It is a genus of Acer species of shrubs in the family Aceraceae. A. ginnala grows in Korea, Japan and Mongolia. We accomplished the structure elucidation by confirming that the result of $^1H$,$^{13}C-NMR$,MS spectrum data was similar to previous references. We measured DPPH and ABTS radical scavenging activity in vitro to evaluate anti-oxidative activities on acertannin isolated from A. ginnala. Acertannin from A. ginnala exhibited potent DPPH and ABTS radical scavenging activities. We examined the antioxidant and apoptosis modulative effects. This examination shows that A. ginnala has not only 1,1-diphenyl-2-picryhydrazyl(DPPH) radical scavenging activity and ABTS radical scavenging activity, but also human hair dermal papilla cell protection effects. These results indicate that the barks and xylems of A. ginnala might be developed as a potent anti-oxidant, hair growth agent, and ingredient for related new functional cosmetic materials.

Synthesis of New N2O Tridentate Ligands and Their Stability Constants of Transition Metal Complexes (새로운 N2O계 세 자리 리간드의 합성과 전이금속 착물 안정도상수)

  • Kim, Sun-Deuk;Park, Young-Sik
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.569-577
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    • 2003
  • Ligands, Br-PEMP, Cl-PEMP and $CH_3O-PEMP$ having Br, Cl and $CH_3O$ substituents at 5-position of the $N_2O$ tridentate ligand, 2-[(2-pyridine-2-ethylamio)-methyl]-phenol (H-PEMP) containing pyridine and phenol were synthesized. Another ligand, Naph-PEMP having pyridine and 2-hydroxy-1-naphthalene was also synthesized. The ligands were characterized using elemental analysis, UV-visible, IR, $^1H\;NMR\;and\;^{13}C$ NMR spectroscopy and mass analysis. The potentiometric titration study in aqueous solution revealed that the proton dissociation of the ligands occurred in three steps and the order of overall proton dissociation constants (log${\beta}$) was $CH_3O-PEMP$ > Naph-PEMP > H-PEMP > Cl-PEMP > Br-PEMP. The order of stability constants (logML and log$ML_2$) of their transition metal complexes was Co(II) < Ni(II) < Cu(II) > Zn(II). The order in their stability constants values of each transition metal complex agreed well with that in overall proton dissociation constant value of the ligands.