• 제목/요약/키워드: $^1H-NMR$ Spectrum

검색결과 230건 처리시간 0.029초

압력 감지형 페인트용 발광 센서로 플라티늄포르피린 핵을 갖는 덴드리머의 제조에 관한 연구 (Synthesis of Platinumporphyrin-Core Dendrimers as Luminescent Sensors for Pressure Sensitive Paints)

  • 정연태;허훈
    • 한국인쇄학회지
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    • 제19권1호
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    • pp.17-27
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    • 2001
  • 플라티늄포르피린 핵과 주위에 8, 16, 32 그리고 64 개의 벤질 단위를 갖는 새로운 덴드리머를 압력 감지형 페인트에 사용할 발광체로 합성하였다. 플라티늄포르피린 핵을 갖는 제 1 세대의 덴드리머는 Lindsey형 합성법을 이용하여 제조하였으며, 제 2 세대에서 제 4 세대까지의 플라티늄포르피린 핵을 갖는 덴드리머는 플라티늄 테트라키스(3,5-디히드록시페닐)포르피린을 적합한 덴드론 브로마이드와 Williamson 에테르 합성법에 따라 알킬화반응시켜 제조하였다. 이러한 에테르 연결의 생성 반응들은 $K_2$CO$_3$와 18-크라운-6를 사용하여 아세톤 용매에서 질소 기류 하에서 6$0^{\circ}C$에서 수행하였을 때 가장 좋은 결과를 주었다. 그리고 이렇게 합성한 덴드리머들을 $^1$H-NMR, $^{13}$C-NMR, Mass spectrum 이용하여 구조를 확인하고, 그리고 UV-VIS spectroscopy를 이용하여 분광학적인 특성을 조사하였다.

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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$\%$.

안트라센이 포함된 새로운 호스트 화합물의 합성과 물성 (Synthesis and Fluorescent Properties of New Host Compound Containing Anthracene Moiety)

  • 장승현
    • 한국환경과학회지
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    • 제17권12호
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    • pp.1373-1380
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    • 2008
  • Anthracene appended new host compounds have been synthesized by imine reaction. Fluorescent open chain host compounds Trisanthryl-tris(2-aminoethyl)imine 1 was synthesized from the reaction of tris(2-aminoethyl)amine and anthracene-9-carboxaldehyde in EtOH. Tris-10-chloroanthryl-tris(2-aminoethyl)imine 2 was synthesized from tris(2-aminoethyl)amine and 10-chloro-9-anthraldehyde in EtOH. The structures of all reaction product were identified by $^1H$ NMR, $^{13}C$ NMR, GC/MS, FAB Mass, IR spectrum and DSC. Cation complexation behavior was investigated by fluorescence spectroscopy measurements. The capability of transition metals cation recognition between fluorescent open chain host compound 1, 2 were investigated with $Co^{2+},\;Ni^{2+}\;and\;Cu^{2+}$. The fluorescence intensity was increased by host compounds corresponding guest cations. The relative order of fluorescence intensity changes were $Co^{2+}>Cu^{2+}>Ni^{2+}$. Compound 2 is very sensitive fluorescent sensor of $Co^{2+}$ ion.

토마토로부터 N-nitrosodimethylamine 생성을 억제시키는 유효성분의 검색 (Screening for Components to Inhibit N-Nitrosodimethylamine Formation from Tomato)

  • 최선영;이인숙;이수정;손미예;신정혜;서종권;강민정;성낙주
    • 생명과학회지
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    • 제16권5호
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    • pp.794-798
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    • 2006
  • 토마토 주스를 Sep-pak $C_{18}$ cartridge를 이용하여 ascorbate 및 phenolic 획분으로 분리하여 NDMA 생성 억제 효과를 시험하였다. 시료의 첨가량이 많을수록 NDMA 억제 효과가 비례적으로 증가하여 ascorbate 획분은 최고 $81.37{\pm}0.25%$, phenolic 획분은 $72.03{\pm}0.25%$였다. Phenolic 획분을 prep-HPLC로 4개의 fractions으로 분취하여 NDMA 생성 억제 효과를 실험한 결과 fraction 2에서 활성이 가장 높았으며, fraction 2를 다시 4개의 subfractions으로 재분취하여 활성실험을 한 결과 subfraction 2b의 획분에서 최대 억제율이 pH 1.2에서 $70.62{\pm}0.45%$ 및 pH 4.2에서 $75.30{\pm}0.45%$였다. 그래서 subfraction 2b를 분리, 정제한 후 GC-Mass 및 $^1H-NMR$$^{13}C-NMR$로 동정한 결과 phenolic acid의 일종인 o-coumaric acid임을 확인할 수 있었다.

Separation and Characterization of Water Soluble Blue Pigments Formed from Geniposide of Gardenia Fruits

  • Park, Jee-Eun;Hahn, Tae-Ryong;Paik, Young-Sook
    • Journal of Applied Biological Chemistry
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    • 제44권4호
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    • pp.190-193
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    • 2001
  • Genipin, aglycone of geniposide isolated from fruits of Gardenia jasminoides, was transformed into blue pigments through reaction with glycine and methylamine. The blue pigments formed from glycine-reacted genipin were passed through Bio-Gel P-2 resin yielding fractions GG1 and GG2, and those from methylamine-reacted genipin were separated into fractions GM1-GM4. The first eluted higher molecular-weight fractions, GG1 and GM1, had higher tinctorial strength than the later eluted lower molecular-weight fractions, GG2 and GM2-GM4, respectively. $^1H-NMR$ spectra of GG1 and GM1 showed very broad peaks indicating that structures of the pigments were highly polymeric. $^1H-NMR$ spectra of GG2, GM3, and GM4 showed several sharp peaks at aliphatic and aromatic regions with accompanying broad peaks, although the spectrum of GM2 was rather simple. Determination of the structural and physical nature of the isolated pigments is in progress.

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Structural Characterization of pre-miRNA 155

  • Kim, Won-Je;Shin, JiYeon;Bang, Kyeongmi;Song, Hyun Kyu;Kim, Nak-Kyoon
    • 한국자기공명학회논문지
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    • 제20권2호
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    • pp.46-49
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    • 2016
  • MiRNA-155, upregulated in various cancers, is one of the miRNAs that suppress apoptosis of human cancer. Thus, inhibition of the maturation of miRNA-155 could be an effective way to induce apoptotic cancer cell death. The apical stem-loop of the pre-miRNA-155 has been known as a Dicer biding site for RNA cleavage. Here, to understand the molecular basis of the tertiary interaction between pre-miRNA-155 with Dicer, we characterize the structure of the apical stem-loop of pre-miRNA-155 using NMR spectroscopy. The RNA has a stem-bulge-stem-loop-stem structure, which is consist of G-C Watson-Crick and G-U Wobble base pairs. The assignments of imino- protons were further confirmed by 2D $^{15}N-^1H$ HSQC NMR spectrum. The NMR parameters obtained in this study can be further used to investigate the tertiary interaction between pre-miRNA-155 and other biomolecules such as protein, nucleic acids, or small chemicals which might be used to control the apoptosis of cancer.

$CCl_4$속에서 Thioacetamide의 N-C(S) 부자유회전에 미치는 몇가지 Amide의 영향 (Effect of Some Amides on the Hindered Rotation of N-C(S) Bond of Thioacetamide in $CCl_4$)

  • 노성구;최영상;윤창주
    • 대한화학회지
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    • 제31권6호
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    • pp.486-490
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    • 1987
  • $CCl_4$속에서 티오아세트산아미드(TA)와 몇가지 아미드(N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA) and N,N-dimethylpropionamide (DMP)) 사이의 수소결합이 TA의 N-C(S) 결합 주위의 부자유 회전에 미치는 영향을 nmr 분광학적인 방법으로 연구하였다. $CCl_4$분율이 증가할 때 TA의 $NH_2$기의 양성자 nmr 스펙트럼은 이중선으로 뚜렷하게 분리되었으며, 그 정도는 DMF < DMA < DMP순으로 증가하였다. 이런 현상을 TA와 아미드사이의 분자간 수소결합으로 설명하였다.

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참보라색우무에서 추출한 항균물질의 구조 및 특성 (Structures and some Properties of the Antimicrobial Compounds in the Red Alga, Symphyocladia latiuscula)

  • 임치원;이종수;조영제
    • 한국수산과학회지
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    • 제33권4호
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    • pp.280-287
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    • 2000
  • 참보라색우무는 우리나라 연근해에서 쉽게 채취할 수 있는 미이용 해조류로서 해조류에서 새로운 천연항균성물질을 개발하기 위한 기초자료를 얻을 목적으로 항균성물질을 각종 칼럼을 통하여 분리정제하였으며, MS, NMR spectrum에 의하여 구조를 확인하였고, X선회절분석으로 결정구조를 해석하였다. 또한 이들 물질이 가지는 몇가지 특성을 조사하였다. 참보라색우무 670 g 중에서 최종적으로 세 개의 항균성물질(SL-l, SL-2, SL-3)이 각각 85 mg, 135 mg, 27.7 mg을 얻었다. SL-1 및 SL-2는 MS 및 NMR에 의하여 2,3,6-tribromof,5-dihydroxybenzyl alcohol (MW, 374) ,2,3,6-trib romo4,5-dihydroxybenzyl methyl ether (MW, 388)이였으며, 특히 SL-2를 벤젠-디에틸 에테르 용매중에서 결정화하여 X선 결정 해석에 의하여서도 구조가 확인되었다. 한편 SL-3는 SL-2와 MS 및 carbon NMR spectrum에서 잘 일치하였으나 proton NMR에서 signal의 패턴이 약간 달라 SL-2의 어떤 이성질체라고 추정되었다. 참보라색우무 항균성물질의 마우스에 대한 치사독성은 SL-1은 3 mg, SL-2는 5 mg까지는 별다른 영향을 미치지 않았으며, PhIP 및 MeIQx에 대한 돌연변이원성 억제효과는 SL-1은 $200 {\mu}g/ml$의 농도에서는 $17.8 {\%}$$17.7 {\%}$에 미치지 않았으나SL-2는 $250 {\mu}g/ml$의 농도에서는 높은 억제효과를 나타내어 새로운 보존료로서의 이용가능성을 제시하였다.

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Structural Characterization of a Flavonoid Compound Scavenging Superoxide Anion Radical Isolated from Capsella bursa-pastoris

  • Kweon, Mee-Hyang;Kwak, Jae-Hyock;Ra, Kyung-Soo;Sung, Ha-Chin;Yang, Han-Chul
    • BMB Reports
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    • 제29권5호
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    • pp.423-428
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    • 1996
  • A superoxide anion radical scavenger isolated from Capsella bursa-pastoris was characterized by infrared (IR) spectroscopy, sugar analysis, ultraviolet (UV) spectroscopy, $^{1}H$ and $^{13}C$ nuclear magnetic resonance (NMR) spectroscopies, and fast atom bombardment (FAB) mass analysis. The compound was assumed to be a flavonoid-O-glycoside from IR spectrum and UV absorption maxima. When the sugar composition of the compound was examined by thin layer chromatography (TLC) and gas chromatography (GC) of the acid hydrolysate, only glucose was detected. According to the results of UV spectrotroscopy by using shift reagents, the compound was supposed to be luteolin (5,7,3',4'-tetrahydroxy flavone) or chrysoeriol (5,7,4'-trihydroxy-3'-methoxy flavone) with glucose. Based on $^{1}H$- and $^{13}C-NMR$ spectroscopies, the compound was deduced as 7,4'-dihydroxy-5,3'-dimethoxy-${\alpha}$-6-c-glucosyl-${\beta}$-2"-o-glucosyl flavone. In FAB mass analysis the compound was finally characterized as 7,4'-dihydroxy-5,3'-dimethoxy-${\alpha}$-6-c-glucosyl-${\beta}$-2"-o-glucosyl flavone ($C_{29}H_{34}O_{16}$, M.W.=638).

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새로운 6-Substituted Pyridazin-3(2H)-one 유도체 및 토토머형의 합성 (Synthesis of its Tautomeric Forms and New 6-Substituted Pyridazin-3(2H)-one Analogs)

  • 김채원;박명숙
    • 약학회지
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    • 제57권5호
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    • pp.316-322
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    • 2013
  • The new pyridazinone analogs were synthesized for development of candidates to retain anticancer activity. Various 6-substituted pyridazin-3(2H)-ones were prepared from the pyridazinyl chloride 3a~d via endothermic nucleophilic substitution with hydroxide ion as nucleophile for 2~48 h. Pyridazinyl chloride 3a~d could be converted to hydroxypyridazines (or pyridazin-3(2H)ones) using 1~5 equivalents of water (or 1 equivalent of sodium hydroxide) at reflux in DMF. The tautomerism of lactim form to lactam form was also accomplished in pyridazine derivatives. Formation of pyridazinones 10 was undertaken with stirring using sodium hydroxide at reflux in DMF for 2 h. Synthetic compounds were identified using NMR spectrum.