• 제목/요약/키워드: $^1H$-, $^{14}C$-NMR

검색결과 157건 처리시간 0.021초

Water activation에 기반한 셀룰로오스의 개질 및 특성 (The Effect of Water Activation on Chemical Modification of Cellulose and Characterization)

  • 김해리;남병욱
    • 한국산학기술학회논문지
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    • 제14권2호
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    • pp.977-982
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    • 2013
  • 다양한 종류의 지방산 아실 체인으로 치환된 Cellulose mixed esters(CME)는 재생 가능한 bio-based 폴리머이다. 셀룰로오스 에스터는 생분해성 고분자로써, 분해되지 않는 석유계 플라스틱을 대체할 미래 고분자 소재이다. 본 연구에서는 개질 실험에 앞서 alpha 셀룰로오스를 $40^{\circ}C$의 증류수에 2시간동안 activation하였다. Water-activated 셀룰로오스와, 다양한 불포화 지방산, 무수 아세트산을 $120^{\circ}C$의 lithium chloride/N,N-dimethylacetamide (LiCl/DMAc)용매에서 5시간동안 반응시켜 CME를 합성했다. 세척과 감압을 반복한 후, TGA, FT-IR, 1H-NMR과 FE-SEM를 통해 특성을 관찰하였고, water activation이 셀룰로오스의 수산기 치환에 미치는 영향에 대하여 조사하였다.

소목(Caesalpinia sappan L.)의 에틸아세테이트 분획물이 Streptococcus mutans에 대한 항균활성 및 부착 억제 (Antimicrobial Activities and Adherence Inhibition on Streptococcus mutans by Ethyl Acetate Extract from Caesalpinia sappan L.)

  • 권현정;김용현;한국일;전미애;한만덕
    • 치위생과학회지
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    • 제12권2호
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    • pp.155-162
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    • 2012
  • 본 연구는 소목(Caesalpinia sappan L.)의 6가지 유기용매 분획물 중 IP-3의 항균활성을 및 부착능을 측정하고 다음과 같은 결과를 얻었다. 1. Methanol에 의해 분리된 소목의 항균 물질 수율은 총 4.8%로 나타났으며, 여러 분획물 가운데 EtOAc 분획물(IP-3)에서 3.94%로 가장 높은 수율을 보였다. 2. 소목의 EtOAc 분획물에서 최종 정제된 활성물질은 UV 288.3 nm에서 최대 흡수피크를 나타내었으며, NMR spectrum을 통해 brazilin(($C_{16}H_{14}O_5$)으로 확인되었다. 3. S. mutans에 대한 소목의 EtOAc 분획물의 항균 활성은 최소억제농도(MIC) 3.1 mg/ml에서 균의 생장을 억제하였다. 4. S. mutans 부착억제효과는 하이드록시아파타이트(HA)를 S. mutans와 24 시간 동안 함께 배양한 대조군은 균 부착률이 높게 관찰되었으나, 소목의 EtOAc 분획물을 처리한 군에서는 HA에 S. mutans의 부착이 매우 적게 나타났다. 이상의 결과를 통해, 소목에서 추출된 EtOAc 분획에 존재하는 brazilin이 구강 내 우식원성세균에 강한 항균력을 가지고 있는 것으로 판단되며, 특히 S. mutans의 부착 억제능이 확인되어 우식원성 균주에 대한 생약치료제로 활용이 가능할 것으로 사료된다.

은행종실유의 all $cis-{\Delta}^{5,11,14}-C_{20:3}$ 지방산 존재에 관한 연구 (Studies on the Presence of all $cis-{\Delta}^{5,11,14}-C_{20:3}$ Fatty Acid in the Seed Oils of Ginkgo)

  • 김성진;이경희;김연심;조용계
    • 한국응용과학기술학회지
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    • 제10권1호
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    • pp.57-65
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    • 1993
  • The fatty acid, all $cis-{\Delta}^{5,11,14}-C_{20:3}$, in the Gingko nuts oils, was isolated and, purified by urea-adduct method, silver ion silica gel chromatography and HPLC equipped with reversed phase ${\mu}-Bondapak$ $C_{18}$ column. Its structural elucidation was conducted by IR and $^1H$-, $^{13}C$-NMR technique. The fatty acid composition of seed oils mainly consists of linoleic acid(37.73%), vaccenic acid(18.30%), oleic acid(15.18%), palmitic acid(3.37%), palmitoleic acid(3.37%) and ${\Delta}^5$ NMDB fatty acids(8.50%) in which all $cis-{\Delta}^{5,11,14}-C_{20:2}$ predominates.

백편두의 항산화 물질 분리 및 동정 (Purification and Identification of Antioxidant Compounds from Dolichos lablab L. Seeds)

  • 권남우;김재연;조용범;황방연;김준구;우선희;이문순
    • 한국약용작물학회지
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    • 제27권6호
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    • pp.419-426
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    • 2019
  • Background: This study aimed to identify antioxidant compounds from the seeds of Dolichos lablab L. by bioassay-guided isolation and recrystallization. Methods and Results: The water layer of D. lablab L. seed extract inhibits intracellular reactive oxygen species (ROS) expressing the 2',7'-dichlorofluorescein diacetate (DCF-DA), Cu/Zn superoxide dismutase (SOD) and catalase genes, as determined by quantitative real-time PCR (qRT-PCR). Two compounds were purified from the water layer of the seeds of D. lablab L. using column chromatography and prep-high performance liquid chromatography (HPLC). Using nuclear magnetic resonance (NMR) and electrospray Ionization mass spectrometry (ESI-MS), their chemical structures were identified as 5-[(2-acetyl-2,3-dihydro-1H-indazol-1-yl)carbonyl]-4,5-dihydro-3H-furan-2-one (C14H14N2O4) and stachyose. Conclusions: Two active antioxidant compounds were purified from the seed extract of D. lablab L. seed extract and the structures of these compounds were identified as C14H14O4N2 and stachyose.

Nuclear Magnetic Relaxaon Study of the Organic-Inorganic Hybrid Systems (CnH2n+1NH3)2SnCl6

  • Lee, Kyu-Won;Lee, Cheol-Eui
    • Journal of Magnetics
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    • 제10권2호
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    • pp.63-65
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    • 2005
  • The $^1H$ NMR spin-lattice relaxation in a series of the organic-inorganic hybrid systems $(C_nH_{2n+1}NH_3)_2SnCl_6$ (n = 8, 10, 12, 14) undergoing two successive phase transitions was studied. A discontinuity characteristic of a first order phase transition was observed at the high-temperature conformational transition. Besides, the spin-lattice relaxation rate below the conformational transition temperature was well fitted by four types of molecular motions, from which the chain-length dependence of the activation energies of the molecular groups was obtained.

The Crystal Structure of One Natural Compound Cyclo-(1,10-Docandiamino-11,20-Docanedioic) Amide (1,12-Diazacyclodocosane-2,11-Dione)

  • Wei, Wan-Xing;Pan, Yuan-Jiang
    • Bulletin of the Korean Chemical Society
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    • 제23권11호
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    • pp.1527-1530
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    • 2002
  • 1,12-diazacyclodocosane-2,11-dione was first isolated from a plant Phyllanthus niruri Linn. Its structure has been determined by means of spectroscopy methods and X-ray crystallography. Two peptide groups in the big ring (lactam) are the main factors influencing intermolecular contacts. The hydrogen-bond interaction of these hydrophilic groups is observed in the crystal structure. Meanwhile, C-H···O hydrogen bonds in molecules contribute to the formation of the whole crystal. These two kinds of hydrogen-bond form six- member rings among molecules. This compound crystallizes in the triclinic space group P-1 with a= 9.588(1) $\AA$, b= $9.850(1)\AA$, c = $11.810(1)\AA$, $\alpha=$ 68.18(1)$^{\circ}C$ , $\beta=$ 84.98(1), $\gamma$ = 86.03(1)$^{\circ}C$ , V = $1030.66(17)\AA3$ , Z = 2. A disorder of five-member carbon chain in the whole ring is observed in the title compound. The bond angle 105.8(4) is determined for a extreme configuration C(14)-C(15)-C(16), and 117.7(10) for another extreme configuration C(14')-C(15')-C(16'). In this crystal, two molecules are tied each other by short intermolecular hydrogen bonds, the oxygen atom being tied by hydrogen bond to nitrogen atom of another two molecules. The NMR and IR spectral data coincides to the structure of the compound.

Structure elucidation of a newly isolated saponin from Clerodendrum serratum (L) Moon

  • Bhujbal, Santosh S.;K.Nanda, Rabindra;S.Deoda, Ramesh;Kumar, Dinesh;Kewatkar, Shailesh M.;S.More, Laxmikant;J.Patil, Manohar
    • Advances in Traditional Medicine
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    • 제10권4호
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    • pp.319-321
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    • 2010
  • Plant saponins are widely distributed amongst plants and have a wide range of biological properties. Icosahydropicenic acid, $C_{51}H_{80}O_{19}$ ((4S,6bS)-8a-((4,5-dihydroxy-6-methyl-3-((3R)-3,4,5-trihydroxy-6-methyl-tetrahydro-2H-pyran-2-yloxy)-tetrahydro-2H-pyran-2-yloxy)carbonyl)-2-hydroxy-4, 6a, 6b, 11, 14b-pentamethyl-11-(2-methylprop-1-enyl)-3-(3,4,5-trihydroxy-6-(hydroxymethyl) - tetrahydro-2Hpyran-2-yloxy)-1, 2, 3, 4, 4a, 5, 6, 6a, 6b, 7, 8, 8a, 9, 10, 11, 12, 12a, 14, 14a, 14b-icosahydropicene-4-carboxylic acid), a new saponin was first time isolated from the roots of Clerodendrum Serratum (L) Moon (Verbenaceae). The structure elucidation of the compound was carried out by $^1H$ NMR and DART-MS studies.

Cynanchum wilfordii의 성분함량 분석 (Quantitative analysis of Cynanchum wilfordii Hemsley)

  • 이혜원;박소영;이아영;채성욱;최고야;추병길;김호경
    • 한국한의학연구원논문집
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    • 제14권1호
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    • pp.107-111
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    • 2008
  • Objectives : Cynanchum wilfordii(Asclepiadaceae) has been traditionally used as a tonic, the prevention and treatment of various geriatric diseases in Korea. Acetophenone derivatives from C. wilfordii showed neuroprotective activity. In this study, two acetophenones were isolated and quantitative determination of acetophenones from C. wilfordii has been developed for quality stand. Methods : Three acetophenone derivatives were isolated from methanol extract of C. willfordii by the chromatographic separation. Their structures were identified as cynandione A, 2,5-dihydroxy acetophenone and cynanchone A on the basis of spectral data(MS, $^1H-NMR$, $^{13}C-NMR$) and chemical analysis. HPLC analysis was performed to determine the contents of cynandione A and 2,5-dihydroxyacetophenone in C. wilfordii. Results : According to the results, the contents of cynandione A and 2,5- dihydroxyacetophenone were 0.274%, 0.035% by HPLC, respectively. Conclusions : In these results, we have determined the contents of cynandione A and 2,5-dihydroxyacetophenone in Cynanchum wilfordii, respectively. We hope that this study will contribute to the standardization and quality control of herbal medicine.

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Synthesis and Characterization of Poly(fluorenylenevinylene-terphenylenevinylene) Containing Phenyl Pendant Group

  • Kim Yun-Hi;Jung Sung-Ouk;Lee Kwang-Hoi;Kwon Soon-Ki
    • Macromolecular Research
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    • 제14권1호
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    • pp.81-86
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    • 2006
  • Poly(fluorenylenevinylene-terphenylenevinylene) containing phenyl pendant group was synthesized by Suzuki coupling reaction and characterized by ${1}^H$-NMR, ${13}^C$-NMR, and IR-spectrum. The weight average molecular weight ($M_{w}$) of the obtained polymer was 31,000 with a polydispersity index of 1.9. The polymer showed good solubility in common organic solvents, and the solution and film emitted blue emission ($\lambda_{max}$=460 nm) on irradiation with UV light. The ITO/PEDOT/polymer/Al device fabricated using the polymer as an emitting layer emitted blue light with a maximum peak around 460 nm. The maximum efficiency of the device was 0.011$\%$.

Synthesis of Alkylidyne Complexes of Br$(CO)_2(tmeda)M{\equiv}CC_{6}H_{4}Me$ (M = Cr, Mo, W). Crystal Structure of Br$(CO)_2(tmeda)M{\equiv}CC_{6}H_{4}Me$

  • Park, Joon T.;Cho, Jeong-Ju;Suh, Il-Hwan;Lee, Jin-Ho;Lim, Sung-Su;Ryu, Bo-Young
    • Bulletin of the Korean Chemical Society
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    • 제14권2호
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    • pp.266-271
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    • 1993
  • The reaction of $(CO_5$)M=C(OMe)Tol (M=Cr, Mo, W and $Tol=p-C_6H_4Me)$ and $BBr_3$ followed by treatment with tetramethylethylenediamine (TMEDA) yields a mixture of two diastereomers, trans, $cis-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1a), Mo(2a), W(3a)] and cis, $trans-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1b), Mo(2b), W(3b)], respectively. These compounds have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, $^1H$ and $^{13}C-NMR)$ data. The trans, cis-Br(CO)2(tmeda)Cr${\equiv}$CTol (1a), has been examine via a single crystal X-ray diffraction study : $BrCrO_2N_2C_{16}H_{23}$, Mr=407.27, triclinic, $P{\bar{1}},\;a=12.792(2),\;b=13.400(5),\;c= 11.645(4)\;{\AA},\;{\alpha}=101.26(2)^{\circ},\;{\beta}=103.04(2)^{\circ},\;{\gamma}=91.88(2)^{\circ},\;{\nu}=1907(1){\AA}^3,\;Z=2,\;{\rho}(calcd)=1.418\;gcm^{-3},\;{\lambda}(MoK{\alpha})=0.71069\;{\AA},\;{\mu}=26.25 cm^{-1},\;F(000)=831.97,\;T=295K,\;R=0.0977$ for 1332 significant reflections $[F_0>5{\sigma}(F_0)]$. There are two essentially equivalent molecules in the crystallographic asymmetric unit. Each molecule is octahedral with the bromide ligand trans to the alkylidyne carbon, the two cis-carbonyl ligands, and the bidentate TMEDA ligand.