• Title/Summary/Keyword: reductive reaction

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Synthesis of Ibuproxam (Ibuproxam의 합성)

  • 최홍대;마정주
    • YAKHAK HOEJI
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    • v.35 no.2
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    • pp.119-122
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    • 1991
  • A convenient method for the synthesis of ibuproxam, which is a non steroidal antiinflammatory agent, is reported. Friedel-Crafts reaction of isobutylbenzene with ethyl $\alpha$-chloro-$\alpha$-(methylthio)acetate (3) gives ethyl $\alpha$-methylthio-(p-isobutylpheny) acetate (4). Ethyl 2-methylthio-2-(4-isobutylphenyl) propionate (5) is obtained from methylation of the compound (4) with NaH and Mel. lbuproxam (7) is easily synthesized by reductive desulfurization of the compound (5) with zinc dust-acetic acid or Raney nickel, followed by treatment of the resultant ethyl 2-(4-isobutyl-pheny) propionate (6) with H$_{2}$NOH-HCI.

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Synthesis of Butibufen (Butibufen의 합성)

  • 최홍대;마정주
    • YAKHAK HOEJI
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    • v.35 no.2
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    • pp.131-134
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    • 1991
  • A new method for the synthesis of butibufen, which is a non steroidal anti-iriflammatory agent, is described. Friedel-Crafts reaction of isobutylbenzene with ethyl $\alpha$-chloro-.alpha.-(methylthio) acetate (1) gives ethyl $\alpha$-methylthio-(p-isobutylphenyl)acetate (2). Ethyl 2-methylthio-2-(4-isobutylphenyl)butyrate (3) is obtained from treatment of the compound (2) with NaH and Etl. Butibufen (5) is synthesized by reductive desulfurization of the compound (3) with zinc dust-acetic acid or Raney nickel, followed by hydrolysis of the resultant ethyl 2-(4-isobutylphenyl)butyrate (4).

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Selective Dehalogenative Homocoupling of Haloarylsulfonates by th Use of Palladium Catalyst

  • Lee, Tae Su;An, Jeong Ho;Kim, Jin Hwan;Bae, Jin Yeong
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.375-378
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    • 2001
  • The palladium catalyzed dehalogenative homocoupling of haloarylsulfonates under reductive conditions has proceeded selectively depending on the type of the halogen. Thus, an iodo or a bromo leaving group of haloarylsulfonates was homocoupled to gi ve symmetrical biaryls in good yields with the sulfonate group intact, whereas a chloro leaving group gave no reaction under the conditions used. When the more reactive nickel catalyst was employed instead of the palladium catalyst in the reaction, both dehalogenative and desulfonative homocouplings of haloarylsulfonates occurred regardless of the type of the halogen used.

An Efficient Method for the Production of Cyclohexylamine from Cyclohexanone and Ammonia over Cu-Cr-La/γ-Al2O3

  • Qin, Shuanglin;Wang, Pan;Huang, Shuangping;Liu, Shuai;Wang, Gaopeng;Wang, Liping;Sun, Meng;Wang, Xiaoji
    • Journal of the Korean Chemical Society
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    • v.59 no.6
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    • pp.493-498
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    • 2015
  • The reductive amination of cyclohexanone with ammonia over Cu-Cr-a/γ-Al2O3 was investigated. It was found that a proper solvent with high solubility of ammonia and 4Å molecular sieves for the elimination of generated water contributed to the formation of cyclohexylamine in the premixing process. In addition, the addition of ammonia in the fixedbed reactor could obviously improve the conversion of cyclohexanone to cyclohexylamine. Finally, reaction conditions including reaction temperature, hydrogen pressure and charging rate of the premix were optimized. Under the optimized conditions, cyclohexylamine was obtained in 83.06% yield.

Reductive Dissolution of Spinel-Type Iron Oxide by N2H4-Cu(I)-HNO3

  • Won, Hui Jun;Chang, Na On;Park, Sang Yoon;Kim, Seon Byeong
    • Journal of the Korean Ceramic Society
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    • v.56 no.4
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    • pp.387-393
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    • 2019
  • A N2H4-Cu(I)-HNO3 solution was used to dissolve magnetite powders and a simulated oxide film on Inconel 600. The addition of Cu(I) ions to N2H4-HNO3 increased the dissolution rate of magnetite, and the reaction rate was found to depend on the solution pH, temperature, and [N2H4]. The dissolution of magnetite in the N2H4-Cu(I)-HNO3 solution followed the contracting core law. This suggests that the complexes of [Cu+(N2H4)] formed in the solution increased the dissolution rate. The dissolution reaction is explained by the complex formation, adsorption of the complexes onto the surface ferric ions of magnetite, and the effective electron transfer from the complexes to ferric ions. The oxide film formed on Inconel 600 is satisfactorily dissolved through the successive iteration of oxidation and reductive dissolution steps.

Lanthanide-Oxalate Coordination Polymers Formed by Reductive Coupling of Carbon Dioxide to Oxalate: [Ln2(3,5-pdc)2(C2O4)(H2O)4]·2H2O (Ln = Eu, Sm, Ho, Dy; pdc = Pyridinedicarbox

  • Huh, Hyun-Sue;Lee, Soon W.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1839-1843
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    • 2006
  • Hydrothermal reactions of $Ln(NO_3)_3{\cdot}5H_2O $ (Ln = Eu (1), Sm (2), Ho (3), Dy (4)) with 3,5-pyridinedicarboxylic acid (3,5-pdcH2) in the presence of 4,4'-bipyridine led to the formation of the 3-D Ln(III)-coordination polymers with a formula unit of $[Ln_2(3,5-pdc)_2(C_2O_4)(H_2O)_4]{\cdot}2H_2O$. These polymers contain a bridging oxalate ligand ($C_2O_4\;^2$). On the basis of GCMS study of the mother liquor remaining after the reaction, we proposed that the $C_2O_4\;^2$ formation proceeds in three steps: (1) Ln(III)-mediated decarboxylation of $3,5-pdcH_2$ to give $CO_2$, (2) the reduction of $CO_2$ to $CO_2\;^{\cdot}$ by the Ln(II) species, and (3) the reductive coupling of the two $CO_2\;^{\cdot}$ radicals to the oxalate ($C_2O_4\;^2$) ion. All polymers were structurally characterized by X-ray diffraction.

Understanding Deactivation of Ru Catalysts by In-situ Investigation of Surface Oxide Stability under CO Oxidation and Oxidative/Reductive Conditions

  • Qadir, Kamran;Joo, Sang-Hoon;Mun, Bong-Jin S.;Park, Jeong-Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.212-212
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    • 2011
  • In addition to the catalysts' activity and selectivity, the deactivation of catalysts during use is of practical importance. It is crucial to understand the phenomena of the deactivation to predict the loss of activity during catalyst usage so that the high operational costs associated with catalyst replacement can be reduced. In this study, the activity of Ru catalysts, such as nanoparticles (3~6 nm) and polycrystalline thin film (50 nm), have been investigated under CO oxidation and oxidative/reductive reaction conditions at various temperatures with the ambient pressure X-Ray photoelectron spectroscopy (APXPS). With APXPS, the surface oxides on the catalyst are measured and monitored in-situ. It was found that the Ru film exhibited faster oxidation-and-reduction compared to that of nanoparticles showing mild oxidative-and-reductive characteristics. Additionally, the larger Ru nanoparticles showed a higher degree of oxide formation at all temperatures, suggesting a higher stability of the oxide. These observations are in agreement with the catalytic activity of Ru catalysts. The loss of activity of Ru films is correlated with bulk oxide formation, which is inactive in CO oxidation. The Ru nanoparticle, however, does not exhibit deactivation under similar conditions, suggesting that its surface is covered with a highly active ultrathin surface oxide. Since the active oxide is more stable as nanoparticles than as a film, the nanoparticles showed mild oxidative/reductive behavior, as confirmed by APXPS results. We believe these simultaneous observations of both the surface oxide of Ru catalysts and the reactivity in real time enable us to pinpoint the deactivation phenomena more precisely and help in designing more efficient and stable catalytic systems.

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시멘트/슬래그/Fe(II) 시스템에 의한 NAPL TCE의 분해 특성

  • 박정현;강완협;황인성;박주양
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2004.04a
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    • pp.218-222
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    • 2004
  • Batch slurry experiments were conducted to develop cement/slag/Fe(II) system that could treat hazardous liquid wastes containing halogenated organic solvents. Portland cement in combination with Fe(II) was reported to reductively dechlorinate chlorinated organics in a modified solidification/stabilization process. TCE (trichloroethylene) was used a model halogenated organic solvent. The objectives of this study were to assess the feasibility of using cement and steel converter slag amended with Fe(II) as a low cost abiotic reductive dechlorination and to investigate the kinetics of TCE dechlorination over a wide range of TCE concentration. From the result of screening experiments, cement/slag/Fe(II) system was identified as a potentially effective system to treat halogenated organic solvent. Kinetic studies were carried out to further investigate degradation reaction of TCE NAPL (Non Aqueous Phase Liquids) in cement/slag/Fe(II) systems by using batch slurry reactors. Degradation rate of TCE solution in this system can be explained by pseudo-first-order rate law because the prediction with the rate law is in good agreement with the observed data.

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Reductive Dechlorination of Tetrachloroethylene in Soils by Fe(II)-Based Degradative Solidification/Stabilization

  • Hwang, Inseong;Batchelor, Bill
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2001.04a
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    • pp.49-52
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    • 2001
  • An experimental study was conducted to test the feasibility of degradative solidification/stabilization (DS/S) process in treating tetrachloroethylene (PCE) in solid phase systems. The Fe(II)-based ds/s process successfully treated PCE in a soil at the reaction rates that would not allow significant release of the contaminant in the environment. A leach model was also developed that could describe the relative importance of leaching and degradation in ds/s. The first and second Damkohler numbers and dimensionless time were important parameters that determined leaching precesses in wastes treated by ds/s.

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