• 제목/요약/키워드: Carbon 13 NMR

검색결과 132건 처리시간 0.025초

Nitrogen-doped carbon nanosheets from polyurethane foams and removal of Cr(VI)

  • Duan, Jiaqi;Zhang, Baohua;Fan, Huailin;Shen, Wenzhong;Qu, Shijie
    • Carbon letters
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    • 제22권
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    • pp.60-69
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    • 2017
  • Nitrogen-doped carbon nanosheets with a developed porous structure were prepared from polyurethane foams by hydrothermal carbonization following $ZnCl_2$ chemical activation. Scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, solid state $^{13}C$ nuclear magnetic resonance (NMR) spectra and X-ray photoelectron spectroscopy were used to characterize the nitrogen-doped carbon nanosheet structure and composition. The removal of Cr(VI) by the N-doped carbon nanosheets was investigated. The results showed that the maximum removal capacity for chromium of 188 mg/g was found at pH=2.0 with PHC-Z-3. pH had an important effect on Cr(VI) removal and the optimal pH was 2.0. Moreover, amino groups and carboxyl groups in the nitrogen-doped carbon nanosheet played important roles in Cr(VI) removal, and promoted the reduction of Cr(VI) to Cr(III).

Synthesis and Properties of Conjugated Cyclopolymers Bearing Fluorene Derivatives

  • Gal Yeong-Soon;Jin Sung-Ho;Lee Hyo-San;Kim Sang Youl
    • Macromolecular Research
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    • 제13권6호
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    • pp.491-498
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    • 2005
  • Fluorene-containing, spiro-type, conjugated polymers were synthesized via the cyclopolymerization of dipropargylfluorenes (2-substituted, X=H, Br, Ac, $ NO_{2}$) with various transition metal catalysts. The polymerization of dipropargylfluorenes proceeded well using Mo-based catalysts to give a high polymer yield. The catalytic activities of the Mo-based catalysts were found to be more effective than those of W-based catalysts. The palladium (II) chloride also increased the polymer yield of the polymerization. The polymer structure of poly(dipropargylfluorene)s was characterized by such instrumental methods as NMR ($^{1}H_{-}$, $^{13}C_{-}$), IR, UV-visible spectroscopies, and elemental analysis as having the conjugated polymer backbone bearing fluorene moieties. The $^{13}C_{-}$NMR spectral data on the quaternary carbon atoms in polymers indicated that the conjugated cyclopolymers have the six-membered rings majorly. The poly(dipropargylfluorene) derivatives were completely soluble in halogenated and aromatic hydrocarbons such as methylene chloride, chloroform, benzene, toluene, and chlorobenzene. The poly(dipropargylfluorene) derivatives were thermally more stable than poly(dipropargylfluorene) itself, and X-ray diffraction analyses revealed that the polymers are mostly amorphous. The photoluminescence peaks of the polymers were observed at about 457-491 nm, depending on the substituents of fluorene moieties.

Assignment of ¹H and $^{13}C$ Nuclear Magnetic Resonances of Ganglioside $G_{A1}$

  • 이경익;전길자;류경임;방은정;최병석;김양미
    • Bulletin of the Korean Chemical Society
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    • 제16권9호
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    • pp.864-869
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    • 1995
  • Investigation of the structures of the gangliosides has proven to be very important in the understanding of their biological roles such as regulation of differentiation and growth of cells. We used nuclear magnetic resonance spectros-copy in order to investigate the structure of GA1. In order to do this, the assignment of spectra is a prerequisite. Since GA1 does not have polar sialic acid, the spectral overlap is severe. In order to solve this problem, we use 2D NMR spectroscopy and heteronuclear 1H/13C correlated spectroscopy in this study. Here, we report the complete assignment of the proton and the carbon spectra of the GA1 in DMSO-d6-D20 (98:2, v/v). These assignments will be useful for interpreting 1H and 13C NMR data from uncharacterized oligosaccharides and for determining the linkage position, the number of sugar rings, and the sequence of new ganglioside. Amide proton in ring Ⅲ shows many interring nOes and has intramolecular hydrogen bonding. This appears to be an important factor in tertiary folding of GA1. Based on this assignment, determination of three dimensional structure of GA1 will be carried out. Studies on the conformational properties of GA1 may lead to a better understanding of the molecular basis of its functions.

Effects of Reaction pH and Hardener Type on Reactivity, Properties, and Performance of Urea-Formaldehyde (UF) Resin

  • Park, Byung-Dae;Kim, Yoon Soo;So, Won Tek;Lim, Kie Pyo
    • Journal of the Korean Wood Science and Technology
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    • 제30권3호
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    • pp.1-11
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    • 2002
  • This study was conducted to investigate the effects of reaction pH conditions and hardener types on the reactivity, chemical structure and adhesion performance of UF resins. Three different reaction pH conditions, such as traditional alkaline-acid (7.5 → 4.5), weak acid (4.5), and strong acid (1.0), were used to synthesize UF resins which were cured by adding three different hardeners (ammonium chloride, ammonium citrate, and zinc nitrate) to measure adhesion strength. Fourier transform infrared (FT-IR) and carbon-13 nuclear magnetic resonance (13C-NMR) spectroscopies were employed to study chemical structure of the resin prepared under three different reaction pH conditions. Adhesion strength of the resins cured with three different hardeners was determined with lap shear specimens in tension. The gel time of UF resins decreased with an increasing in the amount of both ammonium chloride and ammonium citrate added in the resins. However, the gel time increased for zinc nitrate. Both FT-IR and 13C-NMR spectroscopies showed that the strong reaction pH condition produce uronic structures in UF resin, while both alkaline-acid and weak acid conditions produce quite similar chemical species in the resins. The maximum adhesion strength was occurred with the resin prepared under strong acid pH condition. However, this study indicated that the weak acid reaction condition provide a balance between increasing resin reactivity and improving adhesion strength of UF resin. The measurement of formaldehyde emission from the panels bonded with the UF resins prepared is planned for future work.

핵자기공명분석법을 이용한 수용성 아민 CO2 흡수제인 MEA의 열적변성 분석 (Thermal Degradation of Aqueous MEA Solution for CO2 Absorption by Nuclear Magnetics Resonance)

  • 최정호;윤여일;박성열;백일현;김영은;남성찬
    • 한국수소및신에너지학회논문집
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    • 제27권5호
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    • pp.562-570
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    • 2016
  • At the carbon dioxide capture process using the aqueous amine solution, degradation of absorbents is main factor to reducing the process performance. Also, degradation mechanism of absorbent is important for understanding the environmental risk, route of degradation products, health risk etc. In this study, the degradation products of MEA were studied to clarify mechanism in thermal degradation process. The degradation products were analyzed using a $^1H$ NMR (nuclear magnetic resonance) and $^{13}C$ NMR. The analysis methods used in this study provide guidelines that could be used to develop a degradation inhibitor of absorbent and a corrosion inhibitor.

Structure determination of two new compounds isolated from a marine sponge Haliclona(Gellius) sp.

  • Lee, Kyung;Kim, Yun Na;Jeong, Eun Ju
    • 한국자기공명학회논문지
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    • 제25권2호
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    • pp.24-32
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    • 2021
  • Two new sesterterpenes, including a known sesterterpene, were isolated from the marine sponge Haliclona sp. collected in the Gageo island, Korea. One of the new sesterterpenes (1) was an unusual compound possessing a spiroketal moiety and the other (2) represented a four ring-fused skeleton. The planar structure of compound 1 was identical to gombaspiroketals A and B isolated from the marine sponge Clathria gombawuiensis, but the configuration for the two chiral centers was different each other. On the other hand, the skeletal structure of compound 2 was similar to that of phorone A isolated from Phorbas sp. and a compound from C. gombawuiensis, except for one configuration at C-8. However, in comparing the 1H and 13C NMR spectral data, the proton and carbon chemical shifts for the three compounds were almost consistent. The NOESY spectrum revealed that the C-8 configuration of 2 was reversed to that of the two reported compounds. The configuration for compound 2 was supported by quantum mechanical calculation for the carbon chemical shifts and DP4+ probability for the protons and carbons of 2.

대장균 베타-갈락토시데이즈를 이용하여 합성된 Phenylethanol Galactoside의 NMR Spectroscopy 및 Mass spectrometry (NMR Spectroscopy and Mass Spectrometry of Phenylethanol Galactoside synthesized using Escherichia coli 𝛽-Galactosidase)

  • 이향렬;정경환
    • 한국응용과학기술학회지
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    • 제37권5호
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    • pp.1323-1329
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    • 2020
  • 대장균 효소 𝛽-gal를 이용하여 합성된 phenylethanol galactoside (PhE-gal)의 분자구조를 NMR (1H-와 13C-)과 고성능 mass spectrometry를 이용하여 분석하였다. 그 결과 PhE-gal은 1H NMR에서 2-phenylethanol (PhE)에 갈락토실기가 도입되었음을 나타내는 피크가 나타났다. 방향족 고리에서 오는 𝛿H 7.30~7.21 ppm의 피크와 𝛿H 2.88 ppm에 나타난 벤질기 위치의 CH2에서 오는 피크는 PhE가 존재함을 나타낸다. 지방족 사슬 영역인 𝛿H 4.31 ppm, 4.07 ppm과 𝛿H 3.86~3.38 ppm에서 나타나는 7개의 proton 피크로부터 단당류가 도입되었음을 확인할 수 있었다. 13C NMR 스펙트럼에서 나타난 12개의 탄소 피크 중 4개의 피크는 방향족 고리인 페닐기로부터, 또한 단당류에서 기인한 6개의 탄소피크가 존재하므로 PhE에 단당이 도입되었음을 알 수 있다. PhE-gal의 분자량을 확인하기 위하여 질량분석기로 분석한 결과 m/z가 307.1181인 PhE-gal의 sodium adduct ion ([M+Na]+)이 나타나 생성물이 PhE-gal임을 알 수 있었다. 따라서 본 연구결과 E. coli 𝛽-galactosidase에 의한 촉매반응으로 PhE에 갈락토즈가 첨가된 생성물인 PhE-gal이 성공적으로 생합성 되었음을 확인하였다.

버섯병원균에 대한 길항세균 Bacillus sp. SD-10이 생산하는 항균물질의 분리 (Isolation of Antimicrobial Substance by Produced Bacillus sp. SD-10 with Antagonistic Activity Towards Mushroom Pathogens)

  • 이상원;류현순;갈상완;박기훈;김철호;최영주
    • 생명과학회지
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    • 제14권3호
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    • pp.467-471
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    • 2004
  • Bacillus sp. SD-10이 생산하는 항균물질을 이용하여 버섯의 갈색무늬병균 및 푸른곰팡이병균에 대한 천연물 버섯병해 방제약재 개발을 위한 기초적 연구를 행하였다. Bacillus sp. SD-10은 35∼4$0^{\circ}C$의 배양온도에서 30∼40 hrs 배양하였을 때 가장 높은 항균활성을 나타내었다. 이 배양액을 이용하여 T. virens의 균사 생육저해 및 포자발아 억제 농도를 검토한 결과, 균사생육은 30 ul 이상 처리 시 뚜렷하게 저해되었으며 포자발아는 평판배지에 5%(v/v) 이상 첨가 시 완전하게 억제되었다. Bacillus sp. SD-10의 배양액으로부터 항균물질을 순수분리하여 UPX-1으로 명명하고, UPX-1을 $^1H-$NMR과 $^{13}C$-NMR 스펙트럼으로 구조를 동정한 결과 탄소 6개로 구성된 당 2개가 2당류 구조로 결합되어 있는 화합물임이 밝혀졌다. UPX-1은 T. virens 뿐 아니라 Pse. tolaassi에도 아주 강한 항균효과를 나타내었다.

Synthesis and Characterization of Novel Oxadiazole Derivatives from Benzimidazole

  • Vishwanathan, Balasubramanaya;Gurupadayya, Bannimath
    • 대한화학회지
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    • 제58권5호
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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.

Synthesis and the Absolute Configurations of Isoflavanone Enantiomers

  • Won, Dong-Ho;Shin, Bok-Kyu;Han, Jae-Hong
    • Journal of Applied Biological Chemistry
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    • 제51권1호
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    • pp.17-19
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    • 2008
  • Isoflavanone has been synthesized from the reduction of isoflavone in nearly quantitative yield. Isoflavone with seven equivalents of ammonium formate in the presence of Pd/C in ethanol under $N_2$ atmosphere exclusively produced the two-electron reduced product in two hours. It was characterized by various spectroscopic methods, including UV-VIS, EI-MS, $^1H$-NMR, $^{13}C$-NMR and $^1H$, $^1H$-COSY. The racemic mixture was separated by Sumi-Chiral column chromatography and the absolute configurations of the enantiomers were characterized by circular dichroism spectroscopy.