• Title/Summary/Keyword: $^{13}C-NMR$ data

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A One-Step Synthesis and Antimicrobial Activities of New Substituted Dihydro-1,3,4-Thiadiazoles

  • Mahran, Asma M.;Hassan, Nasser A.
    • Archives of Pharmacal Research
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    • v.29 no.1
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    • pp.46-49
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    • 2006
  • In this study, 2-N-arylimino-2,3-dihydro-1,3,4-thiadiazoles derivatives (6a-h) were synthetized. The mechanism of the studied reactions was discussed. The chemical structures of the compounds were elucidated by their IR, $^1H-NMR,\;^{13}C-NMR$, and Mass spectral data and elemental analyses. The compounds were tested for antimicrobial activity using diffusion agar technique.

Secondary Structure, 1H, 13C and 15N Resonance Assignments and Molecular Interactions of the Dishevelled DIX Domain

  • Capelluto, Daniel G.S.;Overduin, Michael
    • BMB Reports
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    • v.38 no.2
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    • pp.243-247
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    • 2005
  • Dishevelled (Dvl) is a positive regulator of the canonical Wnt signaling pathway, which regulates the levels of $\beta$-catenin. The $\beta$-catenin oncoprotein depends upon the association of Dvl and Axin proteins through their DIX domains, and its accumulation directs the expression of specific developmental-related genes at the nucleus. Here, the $^1H$, $^{13}C$, and $^{15}N$ resonances of the human Dishevelled 2 DIX domain are assigned using heteronuclear nuclear magnetic resonance (NMR) spectroscopy. In addition, helical and extended elements are identified based on the NMR data. The results establish a structural context for characterizing the actin and phospholipid interactions and binding sites of this novel domain, and provide insights into its role in protein localization to stress fibers and cytoplasmic vesicles during Wnt signaling.

Multinuclear Solid-state NMR Investigation of Nanoporous Silica Prepared by Sol-gel Polymerization Using Sodium Silicate

  • Kim, Sun-Ha;Han, Oc-Hee;Kim, Jong-Kil;Lee, Kwang-Ho
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3644-3649
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    • 2011
  • Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

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.

Antioxidative Activity of Flavonoids Isolated from Jindalrae Flowers (Rhododendron mucronulatum Turcz.) (진달래꽃으로부터 분리된 플라보노이드 화합물의 항산화성에 관한 연구)

  • Kim, Mi-Ae;Jones, A. Daniel;Chung, Tae-Yung
    • Applied Biological Chemistry
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    • v.39 no.4
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    • pp.320-326
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    • 1996
  • Seven antioxidative flavonoids were isolated from Jindalrae flowers (Rhododendron mnonulatum Turcz.), an edible plant in Korea. These compounds were identified as afzelin, ampelopsin, catechin, myricetin, myricitrin, quercetin and quercitrin on the basis of IR, UV, FAB-MS, $^1H\;NMR,\;and\;^{13}C\;NMR$ data. These compounds were consisted of two flavonols, three flavonol glycosides, a flavane, and a dihydroflavonol. The flavonol glycosides (14.4 g) present in th ethyl ether and ethyl acetate fractions comprised up to 82% of their total flavonoid amount (17.6 g) finally recovered by means of polyamide C-200 column chromatography, preparative TLC, recrystallization, and Sephadex LH-20 column chromatography. The antioxidant activities were measured in an ethanol solution of linoleic acid in the presence of ferric thiocyanate. The antioxidant efficiency increased in the order of afzrlin<$\alpha-tocopherol$

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Enzymatic Transgalactosylation of Ascorbic Acid by ${\beta}-Galactosidase$ (${\beta}-Galactosidase$에 의한 Ascorbic Acid의 효소적 배당화)

  • Jang, So-Young;Kim, Young-Hoi;Kim, Myung-Kon;Kim, Young-Soo;Hong, Jai-Sik
    • Applied Biological Chemistry
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    • v.41 no.7
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    • pp.500-504
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    • 1998
  • The enzymatic transgalactosylation of L-ascorbic acid was investigated to synthesize a chemically stable form of L-ascorbic acid by using commercially available ${\beta}-galactosidases$. Among various enzymes examined, Aspergillus oryzae ${\beta}-galactosidase$ was found to be formed the derivative of ascorbic acid in a high yield from ascorbic acid and lactose. The reaction product was isolated by ion exchange chromatography on a $Dowex\;1\;{\times}\;8$ (Cl - form) resin and Toyopearl HW-40S gel chromatography. The product was identified as $6-O-{\beta}-_D-galactopyranosyl-_L-ascorbic\;acid$ on the basis of various experimental results, viz., UV, IR, $^1H-NMR,\;^{13}C-NMR$ and mass spectral data.

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Assignment of ¹H and $^{13}C$ Nuclear Magnetic Resonances of Ganglioside $G_{A1}$

  • 이경익;전길자;류경임;방은정;최병석;김양미
    • Bulletin of the Korean Chemical Society
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    • v.16 no.9
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    • pp.864-869
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    • 1995
  • Investigation of the structures of the gangliosides has proven to be very important in the understanding of their biological roles such as regulation of differentiation and growth of cells. We used nuclear magnetic resonance spectros-copy in order to investigate the structure of GA1. In order to do this, the assignment of spectra is a prerequisite. Since GA1 does not have polar sialic acid, the spectral overlap is severe. In order to solve this problem, we use 2D NMR spectroscopy and heteronuclear 1H/13C correlated spectroscopy in this study. Here, we report the complete assignment of the proton and the carbon spectra of the GA1 in DMSO-d6-D20 (98:2, v/v). These assignments will be useful for interpreting 1H and 13C NMR data from uncharacterized oligosaccharides and for determining the linkage position, the number of sugar rings, and the sequence of new ganglioside. Amide proton in ring Ⅲ shows many interring nOes and has intramolecular hydrogen bonding. This appears to be an important factor in tertiary folding of GA1. Based on this assignment, determination of three dimensional structure of GA1 will be carried out. Studies on the conformational properties of GA1 may lead to a better understanding of the molecular basis of its functions.

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.

A sapogenin of randia siamensis

  • Woo, Won-Sick;Choi, Jae-Sue;Tovivich, Phichai
    • Archives of Pharmacal Research
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    • v.7 no.1
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    • pp.57-60
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    • 1984
  • From the roots of Randia siamensis (Rubiaceae), 3${\beta}$, 30-dihydroxy-urs-12en-28-oic acid (30-hydroxy ursolic acid) was isolateed and characterized by spectral data.

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