• Title/Summary/Keyword: One-pot reaction

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Synthesis and Characterization of Zn(1-x)NixAl2O4 Spinels as a New Heterogeneous Catalyst of Biginelli's Reaction

  • Akika, Fatima-Zohra;Kihal, Nadjib;Habila, Tahir;Avramova, Ivalina;Suzer, Sefik;Pirotte, Bernard;Khelili, Smail
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1445-1453
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    • 2013
  • $Zn_{(1-x)}Ni_xAl_2O_4$ (x = 0.0-1.0) spinels were prepared at $800^{\circ}C$ by co-precipitation method and characterized by infrared spectroscopy, X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The specific surface area was determined by BET. SEM image showed nano sized spherical particles. XPS confirmed the valence states of the metals, showing moderate Lewis character for the surface of materials. The powders were successfully used as new heterogeneous catalysts of Biginelli's reaction, a one-pot three-component reaction, leading to some dihydropyrimidinones (DHPMs). These new catalysts that produced good yields of DHPMs, were easily recovered by simple filtration and subsequently reused with persistent activity, and they are non-toxic and environmentally friendly. The optimum amount of catalyst is 20% by weight of benzaldehyde derivatives, while the doping amount has been found optimal for x = 0.1.

Magnetic Nanoparticle Immobilized N-Propylsulfamic Acid as a Recyclable and Efficient Nanocatalyst for the Synthesis of 2H-indazolo[2,1-b]phthalazine-triones in Solvent-Free Conditions: Comparison with Sulfamic Acid

  • Rostami, Amin;Tahmasbi, Bahman;Yari, Ako
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1521-1524
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    • 2013
  • N-Propylsulfamic acid supported onto magnetic $Fe_3O_4$ nanoparticles (MNPs-PSA) was used as an efficient and magnetically recoverable catalyst for synthesis of 2H-Indazolo[2,1-b]phthalazine-1,6,11(13H)-trione derivatives from the three-component, one-pot condensation reaction of phthalhydrazide, aromatic aldehydes and cyclic 1,3-diones, in good to excellent yields at $100^{\circ}C$ under solvent-free conditions. The catalyst was easily separated with the assistance of an external magnetic field from the reaction mixture and reused for several consecutive runs without significant loss of its catalytic efficiency. In order to compare, the synthesis of 2H-Indazolo[ 2,1-b]phthalazine-1,6,11(13H)-trione derivatives in the presence of catalytic amount of sulfamic acid (SA) under same reaction condition was also reported.

One-pot Syntheses of Metallic Hollow Nanoparticles of Tin and Lead

  • Lee, Gae-Hang;Choi, Sang-Il;Lee, Young-Hwan;Park, Joo-T.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1135-1138
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    • 2009
  • Hollow Sn and Pb nanoparticles have been prepared by a rapid injection of an aqueous solution of $SnCl_2$- poly(vinylpyrrolidone) (PVP, surfactant) and $Pb(OAc)_2${\cdot}$3H_2O-PVP$ into an aqueous solution of sodium borohydride (reducing agent) in simple, one-pot reaction at room temperature under an argon atmosphere, respectively. The two hollow nanoparticles have been fully characterized by TEM, HRTEM, SAED, XRD, and EDX analyses. Upon exposure to air, the black Pb hollow nanoparticles are gradually transformed into a mixture of Pb, litharge (tetragonal PbO), massicot (orthorhombic PbO), and $Pb_5O_8$. The order and speed of mixing of the reactants between the metal precursor-PVP and the reductant solutions and stoichiometry of all the reactants are crucial factors for the formation of the two hollow nanocrystals. The Sn and Pb hollow nanoparticles were produced only when 1:(1.5-2) and 1:3 ratios of the Sn and Pb precursors to $NaBH_4$ were employed with a rapid injection, respectively.

Methane Conversion to Hydrogen Using Ni/Al2O3 Catalyst (Ni/Al2O3 촉매를 이용한 메탄의 수소 전환)

  • Kim, Jun-Keun;Park, Joo-Won;Bae, Jong-Soo;Kim, Jae-Ho;Lee, Jae-Goo;Kim, Younghun;Han, Choon
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.466-470
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    • 2008
  • The objective of this study is to convert methane into hydrogen using a nanoporous catalyst in the $CO_2$ containing syngas generated from the gasified waste. For the purpose, $Ni/Al_2O_3$ catalyst was prepared with the one-pot method. According to analyses of the catalyst, three dimensionally linked sponge shaped particles were created and the prepared nanoporous catalysts had larger surface area and smaller particle size and more uniform pores compared to the sphere shaped commercial catalyst. The catalyst for reforming reaction gave the highest $CH_4$ conversion of 91%, and $CO_2$ conversion of 92% when impregnated with 16 wt% of Ni at the reaction temperature of $750^{\circ}C$. At that time, the prepared catalyst remarkably improved the $CH_4$ and $CO_2$ conversion up to 20% compared to the commercial one.

One Pot Synthesis and Characterization of Alginate Stabilized Semiconductor Nanoparticles

  • Sundarrajan, Parani;Eswaran, Prabakaran;Marimuthu, Alexander;Subhadra, Lakshmi Baddireddi;Kannaiyan, Pandian
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3218-3224
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    • 2012
  • Uniform and well dispersed metal sulfide semiconductor nanoparticles incorporated into matrices of alginate biopolymer are prepared by using a facile in situ method. The reaction was accomplished by impregnation of alginate with divalent metal ions followed by reaction with thioacetamide. XRD analysis showed that the nanoparticles incorporated in the polymer matrix were of cubic structure with the average particle diameter of 1.8 to 4.8 nm. Field emission scanning electron microscopy and high resolution transmission electron microscopy images indicated that the particles were well dispersed and distributed uniformly in the matrices of alginate polymer. FT-IR spectra confirmed the presence of alginate in the nanocomposite. The crystalline nature and thermal stability of the alginate polymer was found to be influenced by the nature of the divalent metal ions used for the synthesis. The proposed method is considered to be a simple and greener approach for large scale synthesis of uniform sized nanoparticles.

Total Synthesis of a Norneolignan from Ratanhia Radix

  • Choi, Hong-Daei;Seo, Pil-Ja;Son, Byeng-Wha
    • Archives of Pharmacal Research
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    • v.25 no.6
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    • pp.786-789
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    • 2002
  • The total synthesis of a norneolignan isolated from Ratanhia, 5-(3-hydroxypropyl)-2-(2'-methoxy-4'-hydroxyphenyl)benzofuran (8), is described. The key steps contain the one-pot reaction for a 2-arylbenzofuran 6 from methyl 3-(4-hydroxyphenyl)propionate with 2-chloro-2-methylthio-(2'-methoxy-4'-acetoxy)acetophenone (5) in the presence of $ZnCl_2$, and reductive desulfurization of the resulting product 6.

Positive Charge-doping on Carbon Nanotube Walls and Anion-directed Tunable Dispersion of the Derivatives

  • Shin, Ueon-Sang;Knowles, Jonathan C.;Kim, Hae-Won
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1635-1639
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    • 2011
  • An efficient and novel positive charge-doping on the sidewalls of multi-walled carbon nanotubes has been achieved in the presence of tetrahydrofuran as a dopant and Lewis acidic ionic liquids, [bmim]$Sb_nF_{5n+1}$ (n ${\geq}$ 2; bmim = 1-butyl-3-methylimidazolium), as an activator, leaving air-stable derivatives having positively charged sidewalls and the counter anions, [MWCNT$^{y+}$][SbF$_6^-$]$_y$ (MWCNT = multi-walled carbon nanotube). The derivatization took place very fast in one-pot and under mild reaction conditions. The ionic structure enabled a tunable dissolution of the derivatives in various solvents through anion exchange.

Microwave-induced one-pot Synthesis of Coumarins Using Potassium Dihydrogen Phosphate as a Catalyst Under Solvent-free Condition (무 용매 조건에서 potassium dihydrogen phosphate를 촉매로 사용하는 쿠마린의 마이크로파-유도 단일 용기 내 합성)

  • Niralwad, Kirti S.;Shingate, Bapurao B.;Shingare, Murlidhar S.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.486-489
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    • 2011
  • Potassium dihydrogen phosphate was found to be an efficient catalyst for the Pechmann condensation of phenols with ethyl acetoacetate, leading to the formation of coumarins under microwave-irradiation and solvent-free condition. This procedure offers several advantages, including the low loading of catalysts, high yields, clean reactions, short reaction time for the synthesis of coumarins.

Microwave Assisted One-pot Synthesis of Novel α-Aminophosphonates and heir Biological Activity

  • Rao, Alahari Janardhan;Rao, Pasupuleti Visweswara;Rao, Valsani Koteswara;Mohan, Challamchalla;Raju, Chamarthi Naga;Reddy, Cirandur Suresh
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1863-1868
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    • 2010
  • A simple and efficient synthesis of various $\alpha$-aminophosphonates (3a-l) by the reaction of substituted aromatic/heterocyclic aldehydes, 2-amino-6-methoxy-benzothiazole and dibutyl/diphenyl phosphites under microwave irradiation without catalyst was accomplished. The phosphonates were characterized by elemental analysis, IR, $^1H$, $^{13}C$- and $^{31}PNMR$ spectra. They showed promising antimicrobial, anti-oxidant activities depending on the nature of bioactive groups at the $\alpha$-carbon.

Peptide C-terminal Sequence Analysis by MALDI-TOF MS Utilizing EDC Coupling with Br Signature

  • Shin, Man-Sup;Kim, Hie-Joon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1183-1186
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    • 2011
  • The unique Br signature was utilized for C-terminal amino acid sequencing of model peptides. C-terminal carboxyl group was selectively derivatized in peptides, containing side chain carboxyl group, using 1-ethyl-3-[3-dimethylaminopropyl]carbodiimide hydrochloride (EDC) and Br was introduced using 4-bromophenylhydrazine hydrochloride (BPH) in a one pot reaction. Matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) tandem mass spectra were obtained carrying the Br signature in the y-series ions. The Br signature facilitated C-terminal sequencing and discrimination of C-terminal carboxyl groups in the free acid and amide forms.