• Title/Summary/Keyword: Solvent Free Synthesis

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Ultrasound Mediated, Sodium Bisulfite Catalyzed, Solvent Free Synthesis of 6-Amino-3-methyl-4-substitued-2,4-dihydropyrano[2,3-c]pyrazole-5-carbonitrile

  • Darandale, Sunil N.;Sangshetti, Jaiprakash N.;Shinde, Devanand B.
    • Journal of the Korean Chemical Society
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    • v.56 no.3
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    • pp.328-333
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    • 2012
  • A simple, convenient and practical green synthetic protocol for sodium bisulfite catalyzed multicomponent reaction of ethyl acetoacetate, hydrazine hydrate, malononitrile, and various aldehydes for the synthesis of 6-amino-4-phenyl-3-methyl-2,4-ihydropyrano[2,3-c]pyrazole-5-carbonitriles using ultrasound irradiations in solvent free condition. This method provides the advantage of operational simplicity, shorter reaction time and excellent yields making the protocol environment friendly and economically lucrative.

ZrOCl2·8H2O as an Efficient Catalyst for the Pseudo Four-Component Synthesis of Benzopyranopyrimidines

  • Tavakoli, Hamid Reza;Moosavi, Sayed Mojtaba;Bazgir, Ayoob
    • Journal of the Korean Chemical Society
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    • v.57 no.2
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    • pp.260-263
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    • 2013
  • An efficient and environmentally benign protocol for the pseudo four-component synthesis of benzopyranopyrimidines via condensation of salicylic aldehydes, malononitrile and various amines catalyzed by $ZrOCl_2{\cdot}8H_2O$ as an inexpensive and eco-friendly catalyst with high catalytic activity under solvent-free conditions is reported. This protocol provides a new and improved method for obtaining benzopyranopyrimidines in terms of good yields, simple experimental procedure and short reaction time.

A Novel Method for Synthesis of Bis(indolyl)methanes Using 1,3-Dibromo-5,5-dimethylhydantoin as a Highly Efficient Catalyst Under Solvent-free Conditions

  • Hojati, Seyedeh Fatemeh;Zeinali, Toktam;Nematdoust, Zahra
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.117-120
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    • 2013
  • The reactions of indole with carbonyl groups have been efficiently carried out in the presence of catalytic amounts of 1,3-dibromo-5,5-dimethylhydantoin under solvent-free conditions and corresponding bis(indolyl)-mathanes were obtained in good to excellent yields. Synthesis of di[bis(indolyl)methyl]benzene was also accomplished by this catalyst. Furthermore, chemoselective conversion of aromatic aldehydes to their corresponding bis(indolyl)methanes in the presence of aliphatic aldehydes or ketones was achieved by this method.

A Fast, Highly Efficient and Green Protocol for One-Pot Synthesis of 2,4,5-Trisubstituted Imidazoles Catalyzed by [TBA]2[W6O19] as a Reusable Heterogeneous Catalyst

  • Ashrafi, Mozhgan;Davoodnia, Abolghasem;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1508-1512
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    • 2013
  • A simple and efficient synthesis of 2,4,5-trisubstituted imidazoles was achieved via a one-pot three-component cyclocondensation of benzil, aromatic aldehydes, and ammonium acetate in the presence of a catalytic amount of tetrabutylammonium hexatungstate $[TBA]_2[W_6O_{19}]$ as a heterogeneous catalyst under thermal solvent-free conditions. The key features of this methodology are operational simplicity, high yields, short reaction times, and a recyclable catalyst with a very easy work up.

Synthesis and Application of Solvent-free Waterborne Polyurethane (SWPU) Using Teramethylxylene diisocyanate (TMXDI) (Teramethylxylene diisocyanate (TMXDI)를 사용한 무용제형 수분산 폴리우레탄의 합성 및 응용)

  • Jeong, Boo Young;Cheon, Jung Mi;Yoo, Chong Sun;Chun, Jae Hwan
    • Journal of Adhesion and Interface
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    • v.8 no.4
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    • pp.8-13
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    • 2007
  • In this study, solvent-free waterborne polyurethanes (SWPU) were synthesized with teramethylxylene diisocyanate (TMXDI), poly(tetramethylene glycol) (PTMG) and polycarprolactone (PCL) and different mole ratio of dimethylol proponicacid (DMPA). The effect of ionic contents in the solvent-free waterborn polyurethane on thermal, mechanical properties and adhesion strength were studied. Glass transition temperature (Tg) were in range of $-70{\sim}-50^{\circ}C$ and increased as PCL contents increased in polyol. With more incorporation of PCL and DMPA contents in SWPU, tensile strength, adhesion strength and heat resistance of SWPU increased, while the elongation decreased.

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Preparation, Characterization and First Application of Aerosil Silica Supported Acidic Ionic Liquid as a Reusable Heterogeneous Catalyst for the Synthesis of 2,3-Dihydroquinazolin-4(1H)-ones

  • Yassaghi, Ghazaleh;Davoodnia, Abolghasem;Allameh, Sadegh;Zare-Bidaki, Atefeh;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2724-2730
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    • 2012
  • A new heterogeneous acidic catalyst was successfully prepared by impregnation of silica (Aerosil 300) by an acidic ionic liquid, named 1-(4-sulfonic acid)butylpyridinium hydrogen sulfate [$PYC_4SO_3H$][$HSO_4$], and characterized using FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The amount of loaded acidic ionic liquid on Aerosil 300 support was determined by acid-base titration. This new solid acidic supported heterogeneous catalyst exhibits excellent activity in the synthesis of 2-aryl-2,3-dihydroquinazolin-4(1H)-ones by cyclocondensation reaction of 2-aminobenzamide with aromatic aldehydes under solvent-free conditions and the desired products were obtained in very short reaction times with high yields. This catalyst has the advantages of an easy catalyst separation from the reaction medium and lower problems of corrosion. Recycling of the catalyst and avoidance of using harmful organic solvent are other advantages of this simple procedure.

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.

Three Component Solvent-free Synthesis of Chroman-2,4-dione-based Heterocyclic Ketene Aminal (HKA) Derivatives by "GAP" Chemistry

  • Yu, Fu-Chao;Hao, Xiao-Pan;Jiang, Xiu-Yang;Yan, Sheng-Jiao;Lin, Jun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1625-1632
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    • 2014
  • A concise and efficient one-pot synthesis of chroman-2,4-dione-based HKA derivatives by three component reaction of HKAs, triethoxymethane and 4-hydroxycoumarin derivatives under solvent-free and catalyst-free conditions is described. This protocol has many advantages, in that the GAP (Group-Assistant-Purification) chemistry process is involved in this method. As a result, the experimenter can avoid cumbersome process steps such as traditional chromatography and recrystallization purifications. The desired products can be easily obtained by washing the crude products with 95% EtOH.

Recovery of Cholesterol from the $\beta$-Cyclodexgtrin-Cholestrerol Complex Using Immobilized Cyclomaltodextrinas of Alkalophilic Bacillus sp. KJ 133

  • Kwon, Ho-Jeong;Jung, Hye-Jin;Kwak, Hae-Soo
    • Journal of Microbiology and Biotechnology
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    • v.11 no.4
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    • pp.712-715
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    • 2001
  • A new combined method including the enzymatic hydrolysis of $\beta$-cyclodextrin ($\beta$-CD) and solvent extraction fo cholesterol from the hydrolyzed mixture was developed to recover cholesterol from a $\beta$-CD-cholesterol complex prepared from dairy products, such as cream, milk, and cheese. Cyclomaltodextrinase (cyclomatodextrin dextrin hydrolase, EC 3.2.1.54, DCase_ prepared form alkalophilic Bacillus sp. KJ 133 hydrolyzed the $\beta$-DC of the $\beta$-CD-cholesterol complex, and then, free cholesterol was efficiently extracted from the hydrolyzed mixture by a nonpolar solvent such as ethyl acetate. To increase the stability of free CDase, immobilized CDase was developed using sodium alginate as a carrier. The immobilized CDase showed a high recovery yield of cholesterol in a time-dependent manner compared to the free CDase. A gas chromatography analysis showed that more than 70% of cholesterol was recovered from the $\beta$-DC-cholesterol complex of cream by the immobilized CDase, whereas only 3% and 29% of cholesterol were recovered when the solvent extraction and free CDase treatment were used, respectively. The cholesterol recovered can be used as a raw material for steroid synthesis. Furthermore, this method can be an efficient way to recover cholesterol or other organic compounds that are bound in a $\beta$ -DC-cholesterol or -organic compound complex.

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