• 제목/요약/키워드: $H^1$-NMR spectra

검색결과 409건 처리시간 0.025초

저온저장중 개갑인삼종자내의 생리활성물질 동정 및 변화 (Identification and Changes of Physiologically Active Substances During Chilling Storage of Dehisced Ginseng Seeds)

  • 권우생;백남인;이정명
    • Journal of Ginseng Research
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    • 제21권1호
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    • pp.13-18
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    • 1997
  • Identification and changes of physiologically active substances during chilling storage of dehisced ginseng (Panax ginseng C. A. Meyer) seeds were analyzed using various preparatory separation methods and purification columns; Dowex 50W and silica gel columns. Seven components with Rf values of 0.20, 0.40, 0.58, 0.66, and 0.70 In solvent system, $CHCl_3$:MeOH=3:1 (v/v), Rf values of 0. 63 and 0.74 in solvent system, $CHCl_3$:MeOH:$H_2O$:=7:3:1 (v/v) were obtained through Dowex 50W and silica gel column chromatographies. Two components with Rf values of 0.20 and 0.63 in the all chilling treatments were detected in the extract obtained through both chromatographies, and only the former component was gradually increased till 4 weeks of chilling storage and then rapidly decreased from 8 to 16 weeks. UV spectra of Rf values of 0.66 and 0.56 were similar to that of cytokinin, but their physiological activities were not found. Rf values of 0.20 showed activity by radish cotyledon expansion bioassay. The component with Rf value of 0.20 was revealed to have a naphthalene in the proposed chemical structure by various NMR techniques.

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오동나무꽃의 항암성분 (Cytotoxic Compounds from the Flowers of Paulownia coreana)

  • 오좌섭;지옥표;문형인
    • 생약학회지
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    • 제31권4호
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    • pp.449-454
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    • 2000
  • In search for plant-derived cytotoxic compounds, it was found that the $CHCl_3$ and EtOAC extracts obtained from the flowers of Paulownia coreana Uyeki (Scrophulariaceae) exhibited significant cytotoxic activity against human tumor cell lines, A549, SK-OV-3, SK-MEL-2, XF498, and HCT15. Activity-guided fractionation on the basis of the inhibitory activity against the growth of human tumor cell lines, in vitro, and repeated column chromatography afforded several cytotoxic compounds from P. coreana. The structures and stereochemistry of these compounds were established, on the basis of analysis of spectra including IR, UV, EI-MS, $^{1}H-NMR,\;^{13}C-NMR$ and some chemical transformations, as Compound PCCl $(2-hydroxy-4(15),11(13)-eudesmadien-8{\beta},12-olide)$, Compound $PCC2(2,3-dihydro-4-hydroxy-1(15),11(13)-xanthadien-8{\beta},12-olide)$, Compound PCE1 (chrysophanol), Compound PCE2 (emodin), Compound PCE3 (physcion). Cytotoxic activity of compounds obtained from P. coreana. on five tumor cells lines was evaluated by procedure of SRB methods.

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$^{13}C-^{1}H$ Coupling Constant as a Criterion for the Presence of $\pi$ Bridging in Substituted 9-Benzonorbornenyl Cation

  • Gweon-Young Ryu;Jung-Hyu Shin
    • Bulletin of the Korean Chemical Society
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    • 제14권5호
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    • pp.546-548
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    • 1993
  • The discrete structure of substituted 9-benzonorbornenyl cation 3a and 3c was studied using the empirical ${\Delta}$J equation which was developed by Kelly and coworker$^5$. The ${\Delta}$J values of substituted 9-benzonorbornenyl cations were obtained from p-methyl-6,7-dimethyl benzonorbornen-9-yl (3a) and 9-methyl-6,7-dimethyl benzonorbonen-9-yl (3c) cations under stable ion conditions, and were compared with those of the corresponding ketone analog; these cations were generated by dissolving the corresponding carbinols in superacid at -120$^{\circ}$C and the nmr spectra taken at -60$^{\circ}$C~-90$^{\circ}$C. The ${\Delta}$J values are 8.7 Hz for the bridgehead carbons in cation 3c and 3.1 Hz for cation 3b. The ${\Delta}$J values at C5,8 in fused benzene ring are 14.3 Hz for cation 3c and 8.7 Hz for cation 3a. The excellent correlation of the ${\Delta}$J values with 1$^9F$ chemical shifts of p-fluorophenyl-6,7-dimethylbenzonorbornenyl cation (3d) indicate that ${\Delta}$J value is a reliable probe to charge density at adjacent cationic carbon. These NMR parameters strongly support that the symmetrically ${\pi}$-bridged nonclassical structure (type 2) of substituted 9-benzonorbornenyl cations in stable ion conditions.

저분자량 수용성 키토산이 분급화된 유전자 전달체의 제조 및 특성 (Preparation and Characterization of Low Molecular Weight Water Soluble Chitosan Gene Carrier Fractioned according to Molecular Weight)

  • 장민자;김동곤;정영일;장미경;나재운
    • 폴리머
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    • 제31권6호
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    • pp.555-561
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    • 2007
  • 다양한 분자량을 가진 저분자량 수용성 키토산을 얻기 위해 젖산염이 결합되어 있는 키토산 올리고당을 한외여과막 장치를 이용하여 분리하였고, 새로운 염 제거법으로 유리 아민기를 가진 LMWSC를 제조하였다. 젖산염이 제거된 LMWSC의 특성과 탈아세틸화도가 적외선 분광기(Infrared spectroscopy, IR) 및 핵자기공명장치($^1H-Nuclear$ Magnetic Resonance, $^1H-NMR$)에 의해 확인되었다. 분자량을 나타내는 다분산지수(PDI)는 $1.278{\sim}1.499$로 비교적 좁은 분자량분포를 나타내었다. 유전자 전달체로서의 가능성을 확인하기 위하여, 성공적으로 분자량에 따라 분리된 키토산 올리고당과 염이 제거된 LMWSC의 유전자 전이효율이 293T cell을 이용하여 확인하였다. 또한 유전자 전이효율을 향상시키기 위해 제조된 LMWSC 유도체가 Balb/C mice를 이용하여 평가되었다.

치환기를 가진 질소-산소(N3-O2)계 리간드 합성과 중금속(II)이온 착물의 안정도상수 결정 (Synthesis of Pentadentate Nitrogen-Oxygen(N3-O2) Ligands with Substituents and the Determination of Stability Constants of Their Heavy(II) Metal Complexes)

  • 김선덕;설종민
    • 한국환경과학회지
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    • 제20권6호
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    • pp.687-700
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    • 2011
  • A new $N_3-O_2$ pentadentate ligand, H-BHPT, was synthesized. Hydrochloric acid salts of Br-BHPT, Cl-BHPT, $CH_3O$-BHPT and $CH_3$-BHPT, having Br-, Cl-, $CH_{3-}$ and $CH_3O-$ substituents at the para position of the phenol hydroxyl group of H-BHPT were synthesized. Hydrochloric acid salts of 3OH-BHPT and 4OH-BHPT, having different position of the phenol hydroxyl group of H-BHPT were also synthesized. The synthesis of each ligand was confirmed by C. H. N. atomic analysis and $^1H$ NMR, $^{13}C$ NMR, UV-visible, and mass spectra. The calculated proton dissociation constants ($log{K_n}^H$) of the phenol hydroxyl group and secondary amine group of the synthesized $N_3-O_2$ ligands showed five steps of the proton dissociations. The order of the overall proton dissociation constants ($log{\beta}_p$) of the ligands was Br-BHPT < Cl-BHPT < H-BHPT < $CH_3O$-BHPT < $CH_3$-BHPT. The order agreed with that of Hammett substituent constants (${\delta}_p$). However, dissociation steps of 3OH-BHPT were four and that of 4OH-BHPT was three. The calculated stability constants ($logK_{ML}$) between the ligands and transition metal ions agreed with the order of $log{\beta}_p$ values of the ligands. The order of the stability constants between the transition metal ions with the synthesized ligands was Co(II) < Ni(II) < Cu(II) > Zn(II) > Cd(II) > Pb(II). The order agreed well with that of the Iriving-Williams.

치환기를 가진 질소-산소(N2O2)계 네 자리 리간드의 합성과 중금속(II)이온 착화합물의 안정도상수 결정 (Syntheses of Tetradentate Nitrogen-Oxygen(N2O2)) Ligands with Substituents and the Determination of Stability Constants of Their Heavy(II) Metal Complexes)

  • 김선덕;설종민
    • 한국환경과학회지
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    • 제21권4호
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    • pp.421-435
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    • 2012
  • Novel $N_2O_2$ tetradentate ligands, H-3BPD and H-2BPD were synthesized. Hydrochloric acid salts of Br-3BPD, Cl-3BPD, Br-2BPD and Cl-2BPD having Br and Cl substituents at the $para$ position of the phenol hydroxyl group, were synthesized. The ligands were characterized by C. H. N atomic analysis, $^1H$ NMR, $^{13}C$ NMR, UV-visible, and mass spectra. The proton dissociation constants ($logK_n{^H}$) of the phenol hydroxyl group and secondary amine of the synthesized $N_2O_2$ ligands were shown by four step wise values. The orders of the calculated overall proton dissociation constants ($log{\beta}_p$) were Br-3BPD < Cl-3BPD < H-3BPD in case of 3BPD and Br-2BPD < Cl-2BPD < H-2BPD in case of 2BPD respectively. The order agreed well with that of $para$ Hammett substituent constants(${\delta}_p$). The stability constants($logK_{ML}$) of the complexes between the synthesized ligands and transition metal(II) ions agreed with the order of $log{\beta}_p$ of the ligands. The order of the $logK_{ML}$ value of the each transition metal (II) ion was Co(II) < Ni(II) < Cu(II) > Zn(II) > Cd(II) > Pb(II), which agreed well with that of Iriving-Williams series.

새로운 질소-산소(N3O2)계 다섯 자리 리간드의 합성과 중금속(II) 이온들의 착물 안정도상수에 대한 치환기효과 (Synthesis of New Nitrogen-Oxygen(N3O2) Pentadentate Ligands and the Substituent Effect on the Stability Constants of the Heavy(II) Metal Complexes)

  • 김선덕;이혜원;설종민
    • 한국환경과학회지
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    • 제19권7호
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    • pp.849-860
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    • 2010
  • A new $N_3O_2$ pentadentate ligand, N,N'-Bis(2-hydroxybenzyl)-ethylenetriamine(H-BHET 3HCl) was synthesized. The hydrochloric acid salts of Br-BHET 3HCl, Cl-BHET 3HCl, $CH_3O$-BHET 3HCl and $CH_3$-BHET 3HCl containing Br-, Cl-, H-, $CH_3O-$ and $CH_3-$ groups at the para-site of the phenol group of the H-BHEP were synthesized. The structures of the ligands were confirmed by C. H. N. atomic analysis and $^1H$ NMR, $^{13}C$ NMR, UV-visible and mass spectra. The calculated stepwise protonation constants(${\logK_n}^H$) of the synthesized $N_3O_2$ ligands showed six steps of the proton dissociation. The orders of the overall protonation constants($\log{\beta}_p$) of the ligands were Br-BHET < Cl-BHET < H-BHET < $CH_3O$-BHET < $CH_3$-BHET. The orders agreed well with that of para Hammett substituent constants(${\delta}_p$). The calculated stability constants($\logK_{ML}$) between the ligands and heavy metal ions (Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II)) agreed well with the order of the overall proton dissociation constants of the ligands but they showed a reverse order in para Hammestt substituent constants(${\delta}_p$). The order of the stability constants between the heavy metal ions with the synthesized ligands were Co(II) < Ni(II) < Cu(II) > Zn(II) > Cd(II) > Pb(II).

Thienyl Chalcone 유도체의 가수분해 반응메카니즘과 그 반응속도론적 연구 (The Kinetics and Mechanism of the Hydrolysis to Thienyl Chalcone Derivatives)

  • 황용현;이기창;김진영
    • 한국응용과학기술학회지
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    • 제10권2호
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    • pp.73-80
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    • 1993
  • The hydrolysis reaction kinetics of 2-thienyl chalcone derivatives $[II]{\sim}[V]$ was investigated by ultraviolet spectrophotometery in 20% dioxane-$H_2O$ at $25^{\circ}C$ and the structure of these compounds were ascertained by means of ultraviolet, infrared and NMR spectra. The rate equations which were applied over a wide pH range(pH $1.0{\sim}13.0$) were obtained. The substituent effects on 2-thienyl chalcone derivatives$[II]{\sim}[V]$ were studied, and the hydrolysis were facilitated by electron attracting groups. On the basis of the rate equation, substitutent effect and final product, the plausible hydrolysis reaction mechanism was proposed : At pH $1.0{\sim}9.0$, not relevant to the hydrogen ion concentration, neutral $H_2O$ molecule competitvely attacked on the double bond. By contraries, above pH 9.0, it was proportional to concentration of hydroxide ion.

Isolation of Lipoxygenase Inhibitor from Indonesian Herb

  • Alfi Khatib;Kim, Young-Chan;Chung, Shin-Kyo
    • 한국식품저장유통학회:학술대회논문집
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    • 한국식품저장유통학회 2003년도 춘계총회 및 제22차 학술발표회
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    • pp.111.2-112
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    • 2003
  • A total of 20 extracts derived from different plant family commonly used in Indonesian traditional inflammation medicine were screened for their inhibitory effect on soybean lipoxygenase (SBL) and hyaluronidase (HAse) activity. Three methanol extracts, the bark of Cinnamomum burmanni (CB), the leaves of Piper betel (PB), and fruit of Barringtonia acutangula (BA) were found to have high inhibitory effects, whereas the methanol extract of the leaves of Mimusops elengi (ME) have medium inhibitory effect. The IC50 of CB, PB, BA and ME were found to be 21.7, 16.9, 39.1 and 62.8 g/$m\ell$, respectively. Among the tested extracts, only CB inhibited HAse (IC50 = 27g/$m\ell$). CB was successively fractionated with n-hexane, ethyl acetate, butanol and water. The EtOAc fraction having the strongest activity was fractionated and some compounds were isolated and purified by a preparative HPLC(Develosil ODS-HG-5 column). Coumarin and 2-hydroxy cinnamaldehyde. were identified through the analyses of UV-Vis absorption 1H-NMR, 13C-NMR and FAB+-MS spectra.

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Synthesis and Characterization of Gallium Nitride Powders and Nanowires Using Ga(S2CNR2)3(R = CH3, C2H5) Complexes as New Precursors

  • Jung, Woo-Sik;Ra, Choon-Sup;Min, Bong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제26권1호
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    • pp.131-135
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    • 2005
  • Gallium nitride (GaN) powders and nanowires were prepared by using tris(N,N-dimethyldithiocarbamato)gallium(III) (Ga(DmDTC)$_3$) and tris(N,N-diethyldithiocarbamato)gallium(III) (Ga(DeDTC)$_3$) as new precursors. The GaN powders were obtained by reaction of the complexes with ammonia in the temperature ranging from 500 to 1100 ${^{\circ}C}$. The process of conversion of the complexes to GaN was monitored by their weight loss, XRD, and $^{71}$Ga magic-angle spinning (MAS) NMR spectroscopy. Most likely the complexes decompose to $\gamma$ -Ga$_2$S$_3$ and then turn into GaN via amorphous gallium thionitrides (GaS$_x$N$_y$). The reactivity of Ga(DmDTC)$_3$ with ammonia was a little higher than that of Ga(DeDTC)$_3$. Room-temperature photoluminescence spectra of asprepared GaN powders exhibited the band-edge emission of GaN at 363 nm. GaN nanowires were obtained by nitridation of as-ground $\gamma$ -Ga$_2$S$_3$ powders to GaN powders, followed by sublimation without using templates or catalysts.