• 제목/요약/키워드: NMR spectroscopic analysis

검색결과 204건 처리시간 0.024초

Isolation of Handelin from Chrysanthemum boreale

  • Kang, Sam-Sik;Kim, Ju-Sun;Son, Kun-Ho;Lee, Chong-Ock;Kim, Young-Hee
    • Archives of Pharmacal Research
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    • 제19권5호
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    • pp.406-410
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    • 1996
  • The flowers of Chrysanthemum boreale afforded handelin, a unique guaianolide dimer and a mixture of n-hydrocarbons and n-hydrocarbon alcohols in addition to b-sitosterol and b-sitosterol glucoside. Detailed analysis of the $^{1}H$- and $^{13}C$-NMR spectra of handelin was carried out by the application of two-dimensional $^{1}H-^{1}H$-COSY and $^{1}H$- $^{13}C$ multiple-bond, multiple-quantum spectroscopic correlation techniques. Handelin was inactive in the in vitro anti-tumor activity.

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Synthesis and Spectroscopic Characterization of the New Sitting-atop Complexes from Reaction of Zirconyl Nitrate and Free Base meso-Tetraarylporphyrins in Mild Conditions

  • Dehghani, Hossein;Mansournia, Mohammad Reza
    • Bulletin of the Korean Chemical Society
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    • 제30권8호
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    • pp.1715-1718
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    • 2009
  • A series of sitting-atop (SAT) complexes, [(ZrO)$H_2t(X)pp(NO_3)_2$], have been prepared via the reactions of free base meso-tetraarylporphyrins, $H_2$t(X)pp, with zirconyl nitrate hydrate, ZrO(N$O_3)_2{\cdot}xH_2$O. The products have been characterized by a variety of methods including $^1H\;NMR,\;^{13}C$ NMR, IR and UV-Vis spectroscopies, elemental analysis and conductance measurements. The data indicate that the meso-tetraarylporphyrins coordinate with two pyrrolenine nitrogen atoms to the zirconyl cation located above the distorted porphyrin plane and two protons remain on the pyrrole nitrogens. Such half sandwich-type sitting-atop complexes may be considered as models for the initial steps of the metallation of the macrocycles.

Synthesis and Antibacterial Activity of Novel [3-(4-substitutedphenylamino)-8-azabicyclo [3.2.1] oct-8yl]-phenyl-methanone Derivatives

  • Reddy, B. Surendra;Reddy, A. Babul;Reddy, G. Ramachandra;Reddy, P. Raveendra
    • 대한화학회지
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    • 제55권6호
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    • pp.969-973
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    • 2011
  • The synthesis, as well as spectroscopic and biological studies of a novel class of [3-(4-substitutedphenylamino)-8-azabicyclo [3.2.1] oct-8yl]-phenyl-methanone derivatives are described. All the synthesized compounds were characterized by elemental analysis FTIR, $^1H$-NMR, $^{13}C$ NMR, and Mass spectral data. All the synthesized compounds were exhibit in vitro antibacterial activity.

Cytotoxic Constituents of Diadema setosum

  • Minh, Chau-Van;Kiem, Phan-Van;Huong, Le-Mai;Kim, Young-Ho
    • Archives of Pharmacal Research
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    • 제27권7호
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    • pp.734-737
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    • 2004
  • 5,8-Epidioxycholest-6-en-3-ol (1), cholesterol (2), glycerol 1-palmitate (3) and glycerol 1,3-dioleate-2-stearate (4) were isolated from the methanol extract of the sea urchin Diadema setosum, which was collected from the Halong sea, Vietnam. Chemical structures were established based on extensive 1D, 2D-NMR, FAB-MS, EI-MS spectroscopic data and GC-MS analysis. The NMR spectral data of compound 1 were reassigned by using HMQC and HMBC. Compound 1 was found to have strong cytotoxic effect against various cancer cell lines, such as KB ($IC_{50}$, 2.0 $\mu\textrm{g}$/mL), FL($IC_{50}$, 3.93 $\mu\textrm{g}$/mL), and Hep-2 ($IC_{50}$, 2.4 $\mu\textrm{g}$/mL) by in vitro assay.

제주도 방선균 유래 oxazolomycin 계열 KSM-2690 B의 구조 결정과 항균활성에 관한 연구 (Structure Elucidation and Antibacterial Activity of Oxazolomycin Family KSM-2690 B Derived from Actinomycete Collected in Jeju Island)

  • 정형주;김주영;엄수현;문규호
    • 생약학회지
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    • 제54권1호
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    • pp.16-20
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    • 2023
  • KSM-2690 B (1), a peptide-polyketide hybrid compound, was discovered from an actinomycete strain (CJD 1) isolated from Dong-Baek hill on Jeju Island, Republic of Korea. The chemical structure of 1 was identified by using NMR, MS, and UV spectroscopic analyses. Careful analysis of 1D and 2D NMR data revealed that KSM-2690 (1) has an oxazole ring, a β-lactone-γ-lactam spirocycle ring, and both triene and diene structures. KSM-2690 B (1) showed inhibitory activities against E. coli at 200 ㎍/mL.

A pentacyclic triterpenoid possessing analgesic and anti-inflammatory activities from the fruits of Dregea volubilis

  • Biswas, M.;Biswas, K.;Ghosh, A.K.;Haldar, P.K.
    • Advances in Traditional Medicine
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    • 제9권4호
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    • pp.315-319
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    • 2009
  • In present study evaluate the analgesic and anti-inflammatory activity of the compound obtained from the petroleum ether (40 - 60$^{\circ}C$) extract of the fruits from Dregea volubilis in Swiss albino mice and in Wister albino rats respectively. Dried and crushed fruits of Dregea volubilis were extracted by petroleum ether (40 - 60$^{\circ}C$), the proper solvent system was developed by TLC and subjected to column chromatography for obtaining the pure compound/s. IR, MASS, NMR (PMR, C13 NMR and DEPT) spectroscopic analysis were done to elucidate the structure of the compound/s. The petroleum ether (40 - 60$^{\circ}C$) extract of the fruits of Dregea volubilis led to isolation of a pentacyclic triterpenoid designated as taraxerone and characterized as D- friedoolean- 14- en, 3 one. Taraxerone had been screened for analgesic activity in Swiss albino mice and anti-inflammatory activity in Wister albino rats at the dose of 5 mg/kg body weight orally and exhibit significant analgesic and anti-inflammatory properties.

국내 원자력 발전소 주변 토양 휴믹산의 추출 및 특성 규명 (Isolation and Characterization of Humic Acids Present in the Soils at the Vicinity of Domestic Atomic Power Plants(NPPs))

  • 이창훈;신현상;정근호;조영현;이창우
    • Journal of Radiation Protection and Research
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    • 제28권3호
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    • pp.165-172
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    • 2003
  • 본 연구에서는 국내 원자력발전소가 위치한 지역의 토양(영광, 울진, 고리, 고성, 월성)에 존재하는 휴믹산(HA)을 추출하여 각 시료의 원소성분 및 분광학적 방법(UV/Vis, IR, CPMAS $^{13}C$ NMR)을 이용한 물질 특성을 조사하였고, Aldrich HA과 함께 비교 분석하였다. 분자량 크기 분포의 차이는 한외여과법을 이용하여 조사하였다. 원소분석 결과, 울진 지역의 HA에서 가장 높은 산소 함량비를 보였으며, 고리와 고성지역의 HA에서 상대적으로 낮은 산소 함량비를 보였다(O/C: 0.51(UJHA) vs. 0.43(KRHA), 0.46(KSHA)). 분자량 크기 분포는 울진과 영광 지역의 HA가 고리와 고성 지역의 HA에 비하여 30,000 daltons이상의 고분자가 더 높게 존재함을 알 수 있었다. CPMAS $^{13}C$ NMR, UV/Vis., IR 등의 분광학적 특성분석 결과, 울진과 영광 지역의 HA가 고리, 고성 및 월성 지역의 HA에 비하여 상대적으로 높은 방향족성(aromaticity)과 산소 포함 작용기의 함량이 높은 특성을 보였다. 이상의 결과로 볼 때, 울진과 영광지역의 HA가 상대적으로 더 높은 휴믹화(humification) 단계의 물질 특성을 가짐을 알 수 있었으며, 금속이온과의 반응성이 더 높을 것으로 예측된다.

PET 말단에 대한 인계난연제의 라디칼계 부가반응 (1) - 비스페놀에이비스다이페닐포스페이트의 반응 - (Radical Addition Reaction of Phosphorous based Flame Retardant with End Groups of PET (1) - Reaction of Bisphenol A bis(diphenyl phosphate) -)

  • 김민관;김한도
    • 한국염색가공학회지
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    • 제24권1호
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    • pp.33-38
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    • 2012
  • In this study, to increase flame retardation of poly(ethylene terephthalate) (PET) in burning, bisphenol A bis(diphenyl phosphate) (BDP), a well known flame retardant containing phosphorous, was reacted on end groups of PET by radical pathway. End-capping mechanism of PET with BDP was suggested and confirmed by spectroscopic and thermal analysis. From 400 MHz $^{31}P$ solid state FT-NMR spectrum of end-capped PET (PET-BDP), phosphorus spectra peak in BDP was found at ca. -20 ppm. Furthermore, P-C bond stretching vibration peaks were found ca. $600cm^{-1}$ in FT-IR spectrums of PET-BDP. These results showed that BDP can be chemically added on end groups of PET by our method. Thermal characteristics of pure PET (pPET) and PET-BDP were measured and evaluated by TGA analysis. There was not significant changes in thermal characteristics of PET-BDP compared to that of pPET.

PET 말단에 대한 인계난연제의 라디칼계 부가반응 (2) - 리소시놀비스다이페닐포스페이트의 반응 - (Radical Addition Reaction of Phosphorous based Flame Retardant with End Groups of PET (2) - Reaction of Resorcinol bis(diphenyl phosphate) -)

  • 김민관;손광호;김한도
    • 한국염색가공학회지
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    • 제24권1호
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    • pp.39-44
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    • 2012
  • To improve flame retardation of poly(ethylene terephthalate) (PET) against burning, resorcinol bis(diphenyl phosphate) (RDP), phosphorous containing flame retardant, was incorporated into PET backbone by radical reaction pathway. Radical endcapping of PET with RDP was confirmed by spectroscopic and thermal analysis. From 400 MHz $^{31}P$ solid state FT-NMR spectrum of PET with RDP (PET-RDP), phosphorus spectra peak in RDP was found at ca. -10 ppm. Furthermore, P-C bond stretching vibration peaks were found ca. $530cm^{-1}$ in FT-IR spectrums of PET-RDP. These results indicated that RDP can be chemically bound at the ends of PET by radical addition method. Thermal characteristics of pure PET (pPET) and PET-RDP were measured and evaluated by TGA thermal analysis. There was not significant changes in thermal characteristics of PET-RDP compared to that of pPET.

매립 연령에 따른 침출수중에 존재하는 휴믹물질의 분광학적 특성 분석 (Spectroscopic Characterization of Humic Substances Present in Landfill Leachates with Respect to Landfilling Age)

  • 강기훈;신현상;박희경
    • 대한환경공학회지
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    • 제22권6호
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    • pp.1113-1126
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    • 2000
  • 매립지 침출수에 의한 지하수의 오염으로 생성되는 대수층내 오염대 내에서 휴믹물질이 다른 오염물질의 이동 및 변환에 미치는 영향을 평가하기 위한 기초연구로서 매립지의 매립년한에 따른 침출수중에 존재하는 휴믹물질을 추출하여 그 특성을 분석하였다. 추출된 휴믹물질에 대해 원소분석을 실시하였으며, 분광학적 분석으로서 자외선-가시광선, 적외선, 형광 분광분석과 $^1H$$^{13}C$ 핵자기공명 분석을 실시하였다. 침출수중에 존재하는 휴믹물질은 토양 및 수중으로 부터 추출된 휴믹물질에 비해 구조적으로는 지방족 화합물에 의한 특성이 방향족 화합물에 의한 특성에 비교하여 우세하였으며, 이로부터 침출수 휴믹물질의 휴믹화 정도가 상대적으로 낮음을 알 수 있었다. 한편 매립지의 매립년한이 증가할수록 침출수 휴믹물질의 휴믹화 정도는 증가하는 특성을 보였다.

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