• Title/Summary/Keyword: IR and NMR Spectra

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Synthesis and Characterization of Cobalt(II)/(III), Nickel(II) and Copper(II) Complexes of New 14, 15 and 16-Membered Macrocyclic Ligands

  • El-Tabl, Abdou Saad
    • Bulletin of the Korean Chemical Society
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    • v.25 no.12
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    • pp.1757-1763
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    • 2004
  • A new series of nickel(II), cobalt(II)/(III) and copper(II) complexes of 14, 15 and 16-membered of macrocyclic ligands have been prepared and characterized by elemental analyses, IR, UV-VIS and $^1H-NMR$ spectra, magnetic susceptibilities, conductivities, DTA and ESR measurements. Molar conductances in DMF solution indicate that, the complexes are nonelectrolytes except (9-12) complexes. The electronic spectra show that, all complexes are square planar or distorted octahedral geometry. The ESR spectra of solid complexes (4), (8) and (11) show square planar of axial type symmetry $(d_{x2-y2})$ with considerable covalent bond character. However, complex (12) shows a spectrum of octahedral geometry with $d_{z2}$ ground state. Complex (12) shows exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Structural and Chemical Characterization of Aquatic Humic Substances in Conventional Water Treatment Processes (재래식 정수처리 공정에서 수질계 휴믹물질의 구조 및 화학적 특성분석)

  • Kim, Hyun-Chul;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.1
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    • pp.11-16
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    • 2005
  • Humic substances(HS) from raw and process waters at a conventional water treatment plant were isolated and extracted by physicochemical fractionation methods to investigate their characteristics. They are characterized for their functionality, chemical composition, and spectroscopic characteristics using FT-IR(Fourier transform infrared) and $^1H-NMR$(proton nuclear magnetic resonance) spectroscopy. Humic fraction gradually decreased from 47.2% to 26.4%(from 0.97 to 0.54 mgC/L) through conventional water treatment processes. Concentration of phenolic groups in the HS fraction gradually decreased from 60.5% to 21.8%(from 12.2 to $6.0\;{\mu}M/L$ as phenolic-OH) through water treatment. In the case of carboxylic groups, the concentration increased from 39.5% to 46.9%(from 7.9 to $10.6\;{\mu}M/L$ as COOH) by pre-chlorination, but gradually decreased to 34.2%($9.4\;{\mu}M/L$ as COOH) through sedimentation and sand filtration. From the results of the FT-IR and $^1H-NMR$ spectra of HS, the content of carboxylic groups increased and ratio of aliphatic protons to aromatic protons($P_{Al}/P_{Ar}$) also increased through water treatment, which indicated the increase of aliphatic compounds.

Antioxidative Substance Isolated from the Leaf of Zanthoxylum schinifolium

  • Jeong, Chang-Ho;Shim, Ki-Hwan
    • Preventive Nutrition and Food Science
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    • v.13 no.3
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    • pp.241-244
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    • 2008
  • Methanol extracts were prepared from Z. schinifolium leaf and successively fractionated with chloroform, butanol, and water. The butanol fraction exhibited the highest antioxidative activities. Therefore the butanol fraction was purified and a chemical structure was identified by $^1H-^{13}C-NMR$ spectra, and FT-IR. The isolated antioxidative substance was identified as quercitrin.

Coumarin Components in the Root of Peucedanum terebinthaceum (기름나물 뿌리의 Coumarin 성분)

  • Ryu, Kyung-Soo;Yook, Chang-Soo
    • Korean Journal of Pharmacognosy
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    • v.3 no.4
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    • pp.215-216
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    • 1972
  • Five compounds$(I{\sim}V)$ were isolated from the roots of Peucedanum terebinthacem growing in Korea. Compounds I, IV and V are ${\beta}-sitosterol$, bergapten and umbelliferone, respectively. IR and NMR spectra of compounds II (mp. $190^{\circ}$) and III(mp. $111{\sim}120^{\circ}$), both white needle crystalls, indicate that compounds II is a furocoumarin and that compound III, yielding decursinol upon saponification, is a pyranocoumarin.

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Chlorosmaridione; A Novel Chlorinated Diterpene Quinone Methide from Rosemarinus officinalis L.

  • El-Lakany, Abdalla M.
    • Natural Product Sciences
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    • v.10 no.2
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    • pp.59-62
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    • 2004
  • A novel chlorinated diterpene quinone methide; chlorosmaridione (7-chloro-11-hydroxy-abeita-7,9(11),13-triene-6,12-diode) was isolated from petroleum ether extract of the stems of Rosemarinus officinalis L. growing in Egypt. In addition, ${\beta}-sitosterol$, stigmasterol, lupeol acetate, ${\alpha}-amyrin,\;{\beta}-amyrin$, lupeol, acetyloleanolic acid, acetylursolic acid taxodione, horminone, and cryptotanshinone were also identified. Chemical structures of the isolated compounds have been elucidated on the bases of physical, chemical, and spectral data including IR, UV, MS, 1D-and 2D-NMR spectra.

Photocycloaddition of 5,7-Dimethoxycoumarin to 5-Fluorouracil

  • Shim, Sang-Chul;Ra, Choon-Sup;Chae, Kyu-Ho
    • Bulletin of the Korean Chemical Society
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    • v.1 no.4
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    • pp.121-123
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    • 1980
  • $C_4$-Photocycloaddition of 5,7-dimethoxycoumarin(DMC) to 5-fluorouracil(5-FU) was studied in frozen aqueous solution. The major photoproduct was diagnosed and isolated by TLC and column chromatography. The structure of isolated photoproduct was identified as a $C_4$-cycloaddition product of DMC and 5-FU by the characteristics of its UV, IR, NMR, mass spectra, elemental analysis, and photosplitting.

Studies on the Anti-inflammatory Activity of Aralia continentalis (II)

  • Han, Byung-Hoon;Park, Myung-Hwan;Han, Yong-Nam;Josefina B.Manalo
    • Archives of Pharmacal Research
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    • v.6 no.1
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    • pp.75-77
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    • 1983
  • Two phenolic acids were isolated from the hydrolyzed butanol fraction of Aralia continenetalis K. in crystalline form. They were identified by chemical tests and by analysis of spectra of UV, IR and NMR as ferulic acid and caffeic acid.

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New Cryptand Complexes of Lanthanides(Ⅲ) and Dioxouranium(Ⅵ) Nitrates

  • Oh-Jin Jung;Chil-Nam Choi;Hak-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • v.12 no.2
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    • pp.130-137
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    • 1991
  • The following new cryptand 221 complexes of lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate have been synthesized: $(Ln(C_{16}H_{32}N_2O_5)(H_2O)_2(NO_3)_3\ and \((UO_2)_2(C_{16}H_{32}N_2O_5)(H_2O)_4(NO_3)_4$. These complexes have been identified by elemental analysis, moisture titration, conductivity measurements and various spectroscopic techniques. The proton and carbon-13 NMR as well as calorimetric measurements were used to study the interaction of cryptand 221 with La(Ⅲ), Pr(Ⅲ ), Ho(Ⅲ) and $UO_2(Ⅱ)$ ions in nonaqueous solvents. The bands of metal-oxygen atoms, metal-nitrogen atoms and O-U-O in the IR spectra shift upon complexation to lower frequencies, and the vibrational spectra ({\delta}NMN$) of metal-amide complexes in the crystalline state exhibit lattice vibrations below 300 $cm^{-1}$. The NMR spectra of the lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate complexes in nonaqueous solvents are quite different, indicating that the ligand exists in different conformation, and also the $^1H$ and $^{13}C-NMR$ studies indicated that the nitrogen atom of the ring has greater affinity to metal ions than does the oxygen atom, and the planalities of the ring are lost by complexation with metal ions. Calorimetric measurements show that cryptand 221 forms more stable complexes with $La^{3+}$ and $Pr^{3+}$ ions than with $UO^{22+}$ ion, and $La^{3+}/Pr^{3+}$ and $UO^{22+}/Pr^{3+}$ selectivity depends on the solvents. These changes on the stabilities are dependent on the basicity of the ligand and the size of the metal ions. The absorption band (230-260 nm) of the complex which arises from the direct interaction of macrocyclic donor atoms with the metal ion is due to n-{\delta}*$ transition and also that (640-675 nm) of $UO^{22+}$-cryptand 221 complex, which arises from interaction between two-dioxouranium(Ⅵ) ions in being out of cavity of the ligand ring is due to d-d* transition.

Synthesis of Spiroannulated Dihydrofuran Compounds Utilizing Cerium(IV) Ammonium Nitrate (Cerium(IV) Ammonium Nitrate를 이용한 Spiroannulated 다이하이드로퓨란 화합물의 합성)

  • Kim, Byung-SO
    • Journal of the Korean Society of Industry Convergence
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    • v.5 no.4
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    • pp.385-390
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    • 2002
  • An efficient synthesis of spiroannulated dihydrofurans is achieved from 1,3-dicarbonyl compounds and exocyclic alkenes in the presence of cerium ammonium nitrate(IV) in moderate yields. In the case of entries 3-9, as a single product was seen. Especially, reaction of 15 with methylenecyclohexane afforded the two regioisomeric cyclo adducts 21 and 22. The structures of these adducts were confirmed by IR and NMR-Spectra.

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Iridoid Glycoside(VI) -Studies on the Iridoid Glycoside of Ajuga multiflora Bunge- (이리도이드 배당체(配糖體)(VI) -조개나물의 이리도이드 배당체-)

  • Chung, Bo-Sup;Yoo, Woan-Keun
    • Korean Journal of Pharmacognosy
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    • v.16 no.3
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    • pp.160-164
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    • 1985
  • Ajuga multiflora Bunge is a perennial herb in the family of Labiatae. The iridoid glycoside was isolated from the ethylacetate fraction and the n-butanol fraction of the plant. The structure of the substance was identified as 8-O-acetylharpagide by UV, IR, NMR spectra and several chemical reactions.

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