• Title/Summary/Keyword: C-13 NMR

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Purification and NMR Studies of RNA Polymerase II C-Terminal Domain Phosphatase 1 Containing Ubiquitin Like Domain

  • Ko, Sung-Geon;Lee, Young-Min;Yoon, Jong-Bok;Lee, Weon-Tae
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1039-1042
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    • 2009
  • RNA polymerase II C-terminal domain phosphatase 1 containing ubiquitin like domain (UBLCP1) has been identified as a regulatory molecule of RNA polymerase II. UBLCP1 consists of ubiquitin like domain (UBL) and phosphatase domain homologous with UDP and CTD phosphatase. UBLCP1 was cloned into the E.coli expression vectors, pET32a and pGEX 4T-1 with TEV protease cleavage site and purified using both affinity and gel-filtration chromatography. Domains of UBLCP1 protein were successfully purified as 7 mg/500 mL (UBLCP1, 36.78 KDa), 32 mg/500 mL (UBL, 9 KDa) and 8 mg/500 mL (phosphatase domain, 25 KDa) yielded in LB medium, respectively. Isotope-labeled samples including triple-labeled ($^2H/^{15}N/^{13}C$) UBLCP1 were also prepared for hetero-nuclear NMR experiments. $^{15}N-^{1}H$ 2D-HSQC spectra of UBLCP1 suggest that both UBL and phosphatase domain are properly folded and structurally independent each other. These data will promise us further structural investigation of UBLCP1 by NMR spectroscopy and/or X-ray crystallography.

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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    • v.30 no.3
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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.

A Study on the Chemical Constituents from Marine Sponge Luffariella sp. (해면 Luffariella sp.의 화학적 성분 연구)

  • Park, Sun Ku;Kim, Sung Soo;Park, Jun Dae;Hong, Jung Sun;Kim, In Kyu
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.559-563
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    • 1995
  • The three metabolites, Germacrene alcohol(1), Aaptamine(2) and Hexacyclic terpene(3) were isolated from Marine Sponge Luffariella sp., collected in October 1992, Manado Bay, Sulawesi in Indonesia showed in vitro activity against KB cancer cell line, and structure assignment for 1 was corrected by comparison of their spectral data with the literature $values^1$. Their structure were elucidated by $^1H$, $^13C$ NMR, $^1H$ $^13C$(1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy$(HMQC)^2$, $^1H$ $^13C$(2 and 3 bond) Heteronuclear Multiple Bond Correlation Spectroscopy$(HMBC)^3$, Electron Impact Mass Spectroscopy(EI ms), Ultra-violet Spectroscopy(UV) and Infrared Spectroscopy(IR).

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

  • Lee, Chang-Hoon;Shin, Hyun-Sang;Chung, Kun-Ho;Cho, Young-Hyun;Lee, Chang-Woo
    • Journal of Radiation Protection and Research
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    • v.28 no.3
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    • pp.165-172
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    • 2003
  • Humic acids present in the soils at the vicinity of domestic atomic power plants(NPPs), located in Yeongkwang(YK), Uljin(UJ), Kori(KR), Koseong(KS), Wolseong(WS) area were isolated, and characterized using elemental analysis and UV/Vis, IR, CPMAS $^{13}C$ NMR spectroscopic methods. The characteristics were compared with one another and with commercial humic acid (Aldrich Co.). Molecular size distributions of the humic acids were determined using a stirred cell ultrafiltration technique. The results of elemental analysis showed that soil humic acid from UJ contains higher oxygen content than humic acids from KR and KS (O/C ratios: 0.51 (UJHA) us. 0.45(KRHA), 0.43(KSHA)). The molecular size distribution revealed that the soil humic acids of UJ and YK contained a higher percentage of larger molecules of > 30,000 daltons, compared to those of KR and KS. The spectral features obtained from UV/vis., IR and CPMAS $^{13}C$ NMR showed that the aromatic character and oxygen containing functional groups in the humic acids from UJ and YK were relatively higher than those of KR and KS. These results indicate that the soil humic acids from UJ and YK were in a higher degree of humification, which may suggest higher affinity of the humic acids with radionuclides released in the soil environments.

Coordination Modes and Properties of Ag(I) Complex with N,N,N',N',N''-Pentamethyldiethylenetriamine

  • Chun, In-Sung;Kwon, Jung-Ah;Bae, Myung-Nam;Lee, Sim-Seong;Jung, Ok-Sang
    • Bulletin of the Korean Chemical Society
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    • v.27 no.7
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    • pp.1005-1008
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    • 2006
  • The reaction of $AgClO_{4}$ with acyclic potential tridentate N,N,N',N',N''-pentamethyldiethylenetriamine (pmdeta) has given colorless crystals suitable for X-ray crystallography. The crystal structure ($P2_{1}$/n, a = 14.413(1) $\AA$, b = 25.270(2) $\AA$, c = 16.130(1) $\AA$, b = $103.012(1){^{\circ}}$, V = 5723.7(8) A$\AA^{3}$, Z = 4, R = 0.0349) has been solved and refined. Three silver(I) ions connect four pmdeta ligands to produce discrete complex of $[Ag_3(pmdeta)_4](ClO_4)_3$. A pmdeta ligand is bridged to three silver(I) ions, and three other pmdeta ligands are chelated to each silver(I) center in a tridentate mode. Thus, the product is a rare tri-nuclear silver(I) complex with two different chemical environments. $^{13}C$ NMR and $MAS\;^{13}$C NMR indicate that the tri-nuclear silver(I) complex is not rigid in solution. The contact angles and thermal analyses of the complex are measured and discussed.

Antioxidative Compounds in Extracts of Eleutherococcus senticosus Max. Plantlets (가시오갈피 유식물체 추출물의 항산화 활성물질)

  • Kim, Myong-Jo;Kwon, Yong-Soo;Yu, Chang-Yeon
    • Korean Journal of Medicinal Crop Science
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    • v.13 no.4
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    • pp.194-198
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    • 2005
  • Two antioxidative compounds were isolated from the methanolic extract of Eleutherococcus senticosus Max. plantlets and identified as chlorogenic acid and 1,4-di-o-caffeoyl-quinic acid on the basis of mass spectroscopy, $^1H-NMR$ and $^{13}C-NMR$ data. The DPPH free radical scavenging activities of chlorogenic acid $(RC_{50}\;:\;1.2\;{\mu}g)$ and 1,4-di-o-caffeoyl-quinic acid $(RC_{50}\;:\;0.4\;{\mu}g)$ were more effective than those of ${\alpha}-tocopherol\;(RC_{50}\;:\;12\;{\mu}g)$. Of them, 1,4-di-o-caffeoyl-quinic acid compound were isolated for the first time from this plant.

Synthesis of Ultra High Refractive Index Monomer for Plastic Optical Lens and Its Ophthalmic Lens Preparation (플라스틱 안경렌즈용 초고굴절 모노머 합성 및 이를 이용한 안경렌즈 제조)

  • Jang, Dong Gyu;Kim, Jong Hyo;Lee, Soo Min;Roh, Soo Gyun
    • Journal of Korean Ophthalmic Optics Society
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    • v.13 no.3
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    • pp.1-6
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    • 2008
  • Purpose: Plastic optical monomer materials having ultra high refractive index have an income of the whole quantity from advanced nations to domestic companies which are related to plastic optical lens. It is necessary to develop novel plastic optical lens materials in order to overcome a FTA provision and revitalize a stagnating optical lens industry in the interior optical lens industries. The new plastic optical lens materials against the substitution effect of income should be gradually demanded. This work will be synthesized novel super high refractive monomer resin materials of urethane lens series and studied the properties of optical lens using it. Methods: ETS-4 (2-(2-mercaptoethylthio)-3-{2-[3-mercapto-2-(2-mercaptoethylthio)propyl thio]ethylthio}propane -1-thiol), which is optical lens monomer resin having super high refractive index, was synthesized and identified its structure and property by elemental analysis, EI-MS, TGA, FT-IR spectroscopy, $^1H$ and $^{13}C$ NMR spectroscopies. After mixing evenly from mixed monomer resin and diisocyanate series, it was casting in glass mold. After thermal curing, the obtained optical lenses were measured and compared with the refractive index and Abbe number for studies of their optical properties. Results: We have synthesized the novel ultra high refractive index monomer resin, ETS-4, and have identified its structure and property by elemental analysis, EI-MS, TGA, FT-IR spectroscopy, $^1H$ and $^{13}C$ NMR spectroscopies. The existence of three isomers for EST-4 was identified by $^{13}C$ NMR spectroscopy. The refractive index ($N_d$ at $25^{\circ}C$) of monomer resin in liquid state obtained from the Abbe refractometer was 1.647. The refractive indexes of raw plastic optical lenses prepared from the mixed ETS-4 monomer and diisocyanate series were in the range of 1.656~1.680. Conclusions: Novel super high refractive index plastic optical lens monomer was synthesized and analysed, the optical lenses prepared using it were colorless transparency and excellent properties. It is of utility for the industrialization.

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Synthesis and Antimicrobial Screening of Pyrimidine Annulated Dihydropyrano[2, 3-c]pyrazole Derivatives

  • Hegde, Hemant;Ahn, Chuljin;Waribam, Preeti;Shetty, Nitinkumar S.
    • Journal of the Korean Chemical Society
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    • v.62 no.2
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    • pp.87-92
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    • 2018
  • A series of pyrimidine annulated dihydropyrano[2, 3-c]pyrazole derivatives were synthesized and screened for their antimicrobial activity. The precursor, dihydropyrano[2, 3-c]pyrazole was synthesised under catalyst free condition using PEG-400 as reaction medium which facilitated improved yield compared to base catalyzed reaction. Wide scope of substrates, simple workup procedure and high yield even in the absence of catalyst are the major highlights of the protocol. Dihydropyrano[2, 3-c]pyrazoles on condensation with formic acid formed pyrimidine annulated dihydropyrano[2, 3-c]pyrazole derivatives. All the products are characterized using FTIR, $^1H-NMR$ and $^{13}C-NMR$ spectroscopic techniques. The molecules have shown good to moderate activity as antimicrobial agents when compared to the standard drug ciprofloxacin.

Isolation and structure elucidation of a catechin glycoside with phospholipase $A_2$ inhibiting activity from Ulmi cortex

  • Park, Sunghyouk;Goo, Yang-Mo
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1995.04a
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    • pp.58-58
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    • 1995
  • 식물에서부터 새로운 소염작용제를 개발하기 위하여 여러식물을 대상으로 염증반응의 초기단계에서 중요한 역할을 하는 것으로 알려진 Phospholipase $A_2$에 저해활성을 갖는 물질을 검색하였고 그 중 강한 억제활성을 보인 유근피에서 유효성분을 분리하였다. 유근피의 에칠 아세테이트 분획에 대하여 실리카겔 크로마토그래피, Sephadex LH-20 크로마토그래피, 분취 박막 크로마토그래피를 수행하여 phenol성 -OH기를 갖는 활성성분인 PSH-II-84-1를 분리하였다. $^1$H-NMR 신호의 양상과 짝지움 상수 값에서 분리된 물질은 (+)-catechin 의 당 유도체로 확인되었다. $^{13}$C-NMR 자료를 분석하여 치환된 당은 D-apiofuranose로 확인되었다. 방향족환의 $^{l3}$C-NMR 신호들은 extended Huekel theory를 응용하여 얻은 net charge 계산 값과 상관시켜 할당하였다. 이상의 구조연구 결과 이 물질은 (+)-catechin-7-0-$\beta$-D-apiofuranoside로 밝혀졌다. (+)-catechin-7-0-$\beta$-D-apiofuranoside의 효소억제활성은 Type II Phospholipase $A_2$에 대하여 $IC_{50}$/이 600$\mu$M이었다.다.

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Structural Investigation of the Hydrolysis-Condensation Process of Modified Titanium Isopropoxide

  • Jung, M. W.;Oh, H. J.;Yang, J. C.;Shul, Y. G.
    • Bulletin of the Korean Chemical Society
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    • v.20 no.12
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    • pp.1394-1398
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    • 1999
  • The structures of modified Ti$(OPr^i)_4$ with chelating ligands (L) such as ethylacetoacetate (Etac), acetylacetone (Acac) and methylacetoacetate (Mtac) were identified by using IR, ¹H NMR and $^13C$ NMR spectroscopies, and the octahedral structure was confirmed after modification. The pre-edge peaks of XANES spectra of modified metal alkoxides also denoted the mixture of five-fold and six-fold structures. The EXAFS fitting results showed the local structure around Ti atom after alkoxide modification. The hydrolysis-condensation rates of modified Ti alkoxide with organic additives were investigated by ¹H NMR spectroscopy. The Ti$(OPr^i)_4$ modified by Acac was less reactive toward hydrolysis-condensation reaction than those modified by the other alkoxides, which can be attributed to the stable ligand structure between Ti$(OPr^i)_4$ and Acac. The small particle size of modified Ti$(OPr^i)_4$ sol was obtained when Acac was employed.