• Title/Summary/Keyword: Solvent-free conditions

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Base Catalysed Pyrimidine Synthesis Using Microwave

  • Kidwai, M.;Rastogi, S.;Saxena, S.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.11
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    • pp.1575-1578
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    • 2003
  • An environmentally benign approach for the synthesis of 2-substituted-4,6-diaryl pyrimidines using inorganic solid supports for its catalytic role as well as an energy transfer medium is described. The methodology eliminates the usage of solvent during the reaction. The reaction time is brought down from hours to minutes along with yield enhancement. The rate enhancement and high yield is attributed to the coupling of solvent free conditions with microwaves. Further, the role of base is studied in the reaction and it is concluded that microwave assisted basic alumina catalysed reaction is the best in terms of catalysis as well as reaction time and yield.

Molecular Dynamics Study of the Self-Diffusion Coefficient and Velocity Autocorrelation Function of a Polymer Molecule in Solution

  • Kang, Hong-Seok;Lee, Young-Seek;Ree, Tai-kyue
    • Bulletin of the Korean Chemical Society
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    • v.4 no.5
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    • pp.223-227
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    • 1983
  • A molecular dynamic computer experiment was performed on a system of 108 particles composed of a single polymer chain and solvent molecules. The state considered was in the immediate neighborhood of the triple point of the system. The polymer itself is an analog of a freely jointed chain. The Lennard-Jones potential was used to represent the interactions between all particles except for that between the chain elements forming a bond in the polymer chain, for which the interaction was expressed by a harmonic potential. The self-diffusion coefficient and velocity autocorrelation function (VACF) of a polymer were calculated at various chain lengths $N_p$, and various interaction strengths between solvent molecules and a polymer chain element. For self-diffusion coefficients D, the Einstein relation holds good; as chain length $N_p$ increases the D value decreases, and D also decreases as ${\varepsilon}_{cs}$ (the interaction parameter between the chain element and solvent molecules) increases. The relaxation time of velocity autocorrelation decreases as ${\varepsilon}_{cs}$ increases, and it is constant for various chain lengths. The diffusion coefficients in various conditions reveal that our systems are in a free draining limit as is well known from the behavior of low molecular weight polymers, this also agrees with the Kirkwood-Riesman theory.

Solvent Extraction for the Separation of Pd(II), Pt(IV), Ir(IV) and Rh(III) from 3 M Hydrochloric Acid Solution (3 M의 염산용액에서 팔라듐(II), 백금(IV), 이리듐(IV) 및 로듐(III)의 분리를 위한 용매추출)

  • Nguyen, Thi Hong;Lee, Man Seung
    • Resources Recycling
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    • v.26 no.3
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    • pp.26-31
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    • 2017
  • LIX 63 showed a selectivity for the extraction of Pd(II) over other PGMs, such as Pt(IV), Ir(IV) and Rh(III) from 6 M HCl solution. Moreover, HCl solution has significant effect on the oxidation-reduction reaction between Ir(IV) and LIX 63. Therefore, the applicability of employing LIX 63 for the separation of the 4 PGMs was investigated from 3 M HCl solution. From 3 M HCl solution, only Pd(II) was selectively extracted by LIX 63 and its extraction percentage was higher than from 6 M HCl solution. Extraction of the Pd(II) free raffinate with TBP led to the selective extraction of Pt(IV). After oxidation of Ir(III) with $NaClO_3$ to Ir(IV), extraction of the Pt(IV) free raffinate with Aliquat 336 selectively extracted Ir(IV). For each extraction step, optimum stripping conditions were obtained. By this process, it was possible to separate the 4 PGMs by solvent extraction from 3 M HCl solution.

Antioxidant activities of phenolic compounds from Ziziphus jujuba Mill extract using subcritical water (대추 아임계수 추출물의 폴리페놀 함량 및 산화방지 평가)

  • Ko, Min-Jung;Kwon, Mi-Ri;Chung, Myong-Soo
    • Korean Journal of Food Science and Technology
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    • v.53 no.3
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    • pp.329-333
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    • 2021
  • Subcritical water extraction (SWE) is an eco-friendly extraction method that uses only purified water as a solvent under high temperature and high pressure conditions. In this study, total phenolics, and antioxidant activity were evaluated in Ziziphus jujuba Mill extracts from subcritical water obtained by varying the extraction temperature (110-190℃) and extraction time (1-20 min). Total phenolics was maximized with extraction at 190℃ for 15 min (67.79±3.45 mg gallic acid equivalent/g jujube). The 2,2-diphenyl-1-picrylhydrazyl free radical scavenging activity (48.84±4.74%) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) free radical scavenging activity (84.75±1.15%) were maximal at extraction conditions of 190℃, for 20 min. All jujube extracts prepared using SWE had higher total phenolics and antioxidant activities than extracts prepared using organic solvent extraction (60℃, 120 min), including methanol and ethanol. SWE could be an excellent alternative to organic solvents for extracting phenolics and antioxidant compounds.

Evaluation of Antioxidant Activity of Solvent Fractions of Angelica gigas Root Using TOSC Assay (TOSC 방법을 이용한 참당귀 뿌리 용매분획(Angelica gigas)의 항산화 활성 평가)

  • Lee, Sook-Young;Seo, Young-Bae;Woo, Won-Hong
    • The Journal of Korean Medicine
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    • v.32 no.1
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    • pp.141-150
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    • 2011
  • Objectives: The aim of this study was to elucidate the antioxidant effect of solvent fractions of Angelica gigas root. Methods: The ethanol extract of Angelica gigas root was suspended in water and then partitioned with dichloromethane (MC Fr.), ethyl acetate (EA Fr.) and butanol (BuOH Fr.), sequentially. The antioxidant activities of solvent fractions of Angelica gigas root were evaluated for radical scavenging activity against stable free radicals (2,2-diphenyl-1-picrylhydrazyl) DPPH, hydrogen peroxide and superoxide anion radicals. In addition the antioxidant activities of solvent fractions of Angelica gigas root against peroxyl radicals, hydroxyl radicals and peroxynitrites were determined by the total oxy-radical scavenging capacity (TOSC) assay. Results: Among the solvent fractions of MC Fr., EA Fr., and BuOH Fr., BuOH Fr. was found to have stronger antioxidant activity with $IC_{50}$ values of 59.72, 14.36, 30.96 and $44.75\;{\mu}g/m{\ell}$ on the DPPH radical, nitrite, superoxide anion and hydrogen peroxide, respectively, than BHA used as a positive control. Moreover, specific TOSC values(564.8, 276.4 and 405.5 TOSC/mM) of BuOH fr. against peroxyl radicals, hydroxyl radical and peroxynitrite were 4 times higher than GSH (136.5, 67.4 102.6 TOSC/mM) used as a positive control. Conclusions: These results suggest that the BuOH fr. of Angelica gigas root has a high antioxidant activity and can be useful to develop functional food against oxidative stress conditions.

Efficient and Regioselective Ring-Opening of Epoxides with Alcohols and Sodium Azide by using Catalytic Amounts of GaCl3/Polyvinylpyrrolidone

  • Pourali, Ali Reza;Ghayeni, Samaneh;Afghahi, Fatemeh
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1741-1744
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    • 2013
  • A new polymeric catalyst was prepared by supporting $GaCl_3$ on cross-linked polyvinylpyrrolidone ($GaCl_3$/PVP). This catalyst was employed for efficient and regioselective ring-opening reaction of epoxides by various alcohols under solvent-free conditions at room temperature. In our procedure, this heterogeneous catalyst was used at neutral and mild reaction conditions to afford high yields of ${\beta}$-alkoxy alcohols. Also, regioselective conversion of epoxides to ${\beta}$-azidohydrines was accomplished by sodium azide in MeOH in the presence of $GaCl_3$/PVP at room temperature. $GaCl_3$/PVP is a non-hygroscopic and recoverable catalyst and is easily separated from reaction mixture by a simple filtration and re-used repeatedly. Also, this catalyst has good handling and can be stored for long time without any reducing of its reactivity.

Chemoselective Iodination of Alcohols with CeCl3·7H2O/NaI over SiO2 under Microwave Irradiation

  • Hosseinzadeh, Rahman;Tajbakhsh, Mahmood;Lasemi, Zahra;Sharifi, Ali
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1143-1146
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    • 2004
  • A simple and effective procedure for conversion of primary, secondary, allylic and benzylic alcohols into the corresponding iodides is described using $CeCl_3{\cdot}7H_2O/NaI\;over\;SiO_2$ under microwave irradiation. Benzylic alcohols are selectively converted in the presence of saturated alcohols into their corresponding benzylic iodides under these conditions.

Brønsted Acidic Ionic Liquids as Efficient Catalysts for Clean Synthesis of Carbamatoalkyl Naphthols

  • Tavakoli-Hoseini, Niloofar;Heravi, Majid M.;Bamoharram, Fatemeh F.;Davoodnia, Abolghasem
    • Bulletin of the Korean Chemical Society
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    • v.32 no.3
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    • pp.787-792
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    • 2011
  • Under mild conditions and without any additional organic solvent, synthesis of carbamatoalkyl naphthols could be carried out in the present of two halogen-free Br${\phi}$nsted acidic ionic liquids, 3-methyl-1-(4-sulfonic acid)butylimidazolium hydrogen sulfate and N-(4-sulfonic acid)butylpyridinium hydrogen sulfate. A wide range of aromatic aldehydes easily undergo condensation with $\beta$-naphthol and methyl or benzyl carbamate to afford the desired products of good purity in excellent yields. The present methodology offers several advantages such as a simple procedure with an easy work-up, short reaction times, and excellent yields. The catalysts could be recycled and reused for several times without substantial reduction in their catalytic activities.

Immobilization of L-Lysine on Zeolite 4A as an Organic-Inorganic Composite Basic Catalyst for Synthesis of α,β-Unsaturated Carbonyl Compounds under Mild Conditions

  • Zamani, Farzad;Rezapour, Mehdi;Kianpour, Sahar
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2367-2374
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    • 2013
  • Lysine (Lys) immobilized on zeolite 4A was prepared by a simple adsorption method. The physical and chemical properties of Lys/zeolite 4A were investigated by X-ray diffraction (XRD), FT-IR, Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-vis. The obtained organic-inorganic composite was effectively employed as a heterogeneous basic catalyst for synthesis of ${\alpha},{\beta}$-unsaturated carbonyl compounds. No by-product formation, high yields, short reaction times, mild reaction conditions, operational simplicity with reusability of the catalyst are the salient features of the present catalyst.