• Title/Summary/Keyword: F NMR

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Preparation and Structure of $Re(NC_6F_5)(PPh_3)_2Cl_3 $ ($Re(NC_6F_5)(PPh_3)_2Cl_3 $화합물의 합성 및 구조)

  • 박병규;김영웅
    • Korean Journal of Crystallography
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    • v.7 no.2
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    • pp.113-119
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    • 1996
  • Reaction of Re(O)(PPh3)2Cl3,I, with 2,3,4,5,6-pentafluoroaniline (C6F5NH2), produced Re(NC6F5)(PPh3)2Cl3, II. The product has been characterized by 1H-NMR, elemental analysis, and X-ray diffraction. II crystallizes in the orthorhombic system, space group Pna21 with cell parameters a=18.763Å, b=14.737(2)Å, c=16.707(3)Å, Z=4. Least-square refinement of the structure led to an R(wR2)factor of 0.0455(0.1148) for 3319 unique reflections of I > 2σ(I) and for 174 variables.

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Comparing the Stability of Geometrically rigid Tricyclopropyl Carbinyl Cations by $^{19}$F NMR Spectroscopy

  • Shin, Jung-Hyu;Kim, Kyong-Tae;Shin, Hun-Woo
    • Bulletin of the Korean Chemical Society
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    • v.8 no.3
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    • pp.144-145
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    • 1987
  • The relative stability as function of geometry in the rigid tricyclopropylcarbinyl cations with varied bond angle (${\alpha}$) between the plane of cyclopropane ring and the bond connecting cyclopropane ring to cationic carbon was examined by $^{19}F$ nmr spectroscopy. 7-p-Fluorophenyltricyclo[2.2.2.$0^{2,6}$]octan-7-yl(4) and 8-p-fluorophenyltricyclo[3.2.2.$0^{2,7}$]nonan-8-yl cation (8) were generated from corresponding tertiary alcohols under stable ion conditions, and their $^{19}F$ chemical shifts were compared with those of model compounds such as 7-nortricyclyl cation (3) and tricyclo[3.3.1.$0^{2,7}$]octan-8-yl cation (7). Consequently, it is concluded that the varied orientation of bond angle (${\alpha}$) within in the bisected conformation does not affect degree of the charge delocalization into cyclopropane ring.

Isolation and Identification of Antimicrobial Active Substance from Sophora flavescens Ait. (고삼으로부터 항균활성 물질의 분리 및 구조 동정)

  • Ahn, Eun-Young;Shin, Dong-Hwa;Baek, Nam-In;Oh, Jin-A
    • Korean Journal of Food Science and Technology
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    • v.30 no.3
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    • pp.672-679
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    • 1998
  • The ethanol extract and its chloroform fraction of Sophora flavescens Ait. exhibited growth inhibition on some food poisoning bacteria. The minimum inhibitory concentration of the above extracts were $50{\sim}500\;ppm$ and below 50 ppm Listeria monocytogenes (ATCC 19111, 19112, 19113, 19114, 15313). By silica gel column chromatography twice, antimicrobial active compound S-10-6 was isolated from chloroform fraction of Sophora flavescens Ait. The fraction S-10-6 showed strong growth inhibition at 10 ppm on 5 strains of L. monocytogenes, Bacillus subtilis ATCC 14593 and Staphylococcus aureus KFCC 11764 but Esherichia coli ATCC 25922 was not inhibited at 100 ppm and also confirmed bactericidal effect at 30 and 50 ppm on 5 strains of L. monocytogenes. The antimicrobial compound S-10-6 was identified as kushenol F, a kind of flavanone compound, by EI/MS, $^1H-NMR\;and\;^{13}C-NMR$.

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Antimutagenic Compounds Identified from the Chloroform Fraction of Garlic (Allium sativum) (마늘의 쿨로로포름 분획에서 동정된 항돌연변이 물질)

  • 김소희;김정옥;이숙희;박건영;박희준;정해영
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.20 no.3
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    • pp.253-259
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    • 1991
  • Methanol extract of garlic was fractionated to chloroform and aqueous fractions. The cholorform fraction possessed the highest antimutagenic activity in Salmonella typhimurium TA 100 and TA98, and was further fractionaed into four Allium sativum chromatography fractions (ASC F1, 2, 3 and 4) by column and thin layer chromatographies. The ASC F2 exhibited the higher antimutagenic activity and contained 18 chemical compounds tentatively identifed by GC-MS, NMR and FT-IR. Among the 18 compounds, methyl linoleate was a major compound to exhibit the antimutagenicity.

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Toxic Evaluation and Chromatographic Analysis of Cucurbitacin D and F from Sorbaria sorbifolia (쉬땅나무(Sorbaria sorbifolia) 성분으로서 cucurbitacin D, F의 독성평가 및 정량)

  • Lee, Sang-Myung;Lee, Cheal-Gyu
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.191-195
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    • 2001
  • Cucurbitacin D and F, the protostane type triterpenoid of S. sorbifolia, were isolated with chromatograpic method and used as the standard substances for quantitative analysis. The compounds were identified with $^1H$-NMR, FAB-MS and UV spectrophotometer. They were separated on YMC-Pack ODS-AQ(303)[$250{\times}4.6mm$ I.D., $S-5{\mu}m$, 120A] column by HPLC. Cucurbitacin F was detected at 10.73mg/kg in cortex of S. sorbifolia, but cucurbitacin D was not. The compounds were shown to exihibit significant cytotoxicity($ED_{50}$<$0.1{\mu}g/mL$) against several tumor cell lines and acute toxicity(cucurbitacin D: 4.7mg/kg/day, cucurbitacin F: 2.5mg/kg/day) against BDF-1 mouse.

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Preparation of Trifluoroacetyl Chitosan Derivatives with Antiviral Activity (항바이러스 활성을 갖는 Trifluoroacetyl Chitosan 유도체의 제조)

  • Kim, Chun-Ho;Shin, Cha-Gyun;Shin, Kye-Sook;Son, Tae-il
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.599-602
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    • 1999
  • Chitosan was depolymerized by using nitrous acid. In order to synthesize new fluorinated chitosan oligomer(FCO) derivative, free amine groups of resulting low molucular weight chitosan oligomers were reacted with trifluoroacetic anhydride. The structure changes in the samples were conformed by using FT-IR, $^{1}H\;NMR$, $^{13}C\;NMR$ and $^{19}F\{^{1}H\}NMR$. Antiviral activity of FCO was studied by measuring DAN amounts of the replication viruses at 36 hr after the cells were infected with the viral solution containing FCO of various concentrations. The viral replications in the cells infected with the viral solution containing FCO were proportionally decreased with the FCO does, compared to those of the control groups, indicating that FCO efficiently inhibits viral infection. In particular, viral replication was decreased to 40% in the 1% FCO-treated cells.

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$^{15}$N NMR Relaxation Study of the Catalytic Residues in Y14F Mutant Ketosteroid Isomerase

  • Yoon, Ye-Jeong;Lee, Hyeong-Ju;Kim, Chul;Lee, Hee-Cheon
    • Journal of the Korean Magnetic Resonance Society
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    • v.8 no.2
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    • pp.77-85
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    • 2004
  • $^1$H-detected $^{15}$N NMR was employed to investigated the effect of mutation (Y14F) on the dynamic properties of catalytic residues in ${\Delta}^5$-3- ketosteroid isomerase (KSI) from Conamonas testosteroni. In particular, the backbone dynamics of the catalytic residues have been studied in free enzyme and its complex with a steroid ligand, 19-nortestosterone hemisuccinate, by $^{15}$N relaxation measurements. The relaxation data were analyzed using the model-free formalism to extract the model-free parameters (S$^2$, ${\tau}_e$, and R$_{ex}$). The results show that the mutation causes a significant decrease in the order parameter (S$^2$) for the catalytic residues of free Y14F KSI, presumably due to breakdown of the hydrogen bond network by mutation. In addition, the order parameters of Phe-14 and Asp-99 increased slightly upon ligand binding, indicating a slight restriction of the high-frequency (pico- to nanosecond) internal motions of the residues in the complexed Y14F KSI, while the order parameter of Tyr-55 decreased significantly upon ligand binding.

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Anti-cancer Activity of Styrax japonica Bark Extrats (때죽나무(Styrax japonica) 수피 추출물의 항암 활성)

  • Kwon, Oh-Woong;Kim, Woo-Jin;Lee, Hak-Ju
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.1
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    • pp.68-77
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    • 2014
  • A compound has been isolated from the methanol extract of Styrax japonica bark using conventional chromatographic methods including silica gel chromatography, TLC and HPLC. The molecular formula of Styraxlignolide F analyzed by spectrometric analyses using FAB-MS, NMR was found to be $C_{27}H_{34}O_{11}Na$. The cytotoxicity of the styralignolide F was showed 15.2% in $1.0mg/m{\ell}$ on human kidney cell (HEK 293). As anticancer activity of $CH_2Cl_2$ fraction, over 60% of AGS and MCF-7 cells were inhibited in concentration of $1.0mg/m{\ell}$. In the results of anticancer test using quantification of Bcl-2, $CH_2Cl_2$ fraction showed lower Bcl-2 and p53 expression than those of styraxlignolide F and other fractions. In apoptosis of human lung carcunoma cancer cell (A549), $CH_2Cl_2$ fraction showed the highest inhibition rate (46.9%) and styralignolide F was the next (43.5%). The $CH_2Cl_2$ fraction showed higher anti-cancer activities than isolated substance (styraxlignolide F), probably due to the crude extract showing synergic effects by other components.