• Title/Summary/Keyword: Solvent Free Synthesis

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An Improved Protocol on the Synthesis of Thiazolo[3,2-a]pyrimidine Using Ultrasonic Probe Irradiation

  • Tan, Sian Hui;Chuah, Tse Seng;Chia, Poh Wai
    • Journal of the Korean Chemical Society
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    • v.60 no.4
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    • pp.245-250
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    • 2016
  • An improved protocol on the synthesis of thiazolo[3,2-a]pyrimidine-6-carboxylate derivatives are reported. Previously, the thiazolo[3,2-a]pyrimidine-6-carboxylate derivatives were prepared in a two-step procedure. Under the improved procedure, the thiazolo[3,2-a]pyrimidine-6-carboxylate derivatives was readily prepared in a one-step reaction. This procedure was found to be more efficient than the previous protocol and also compared to the ultrasound bath and conventional heating methods in terms of yield and reaction time.

Solid-State Ball-Mill Synthesis of Prussian Blue from Fe(II) and Cyanide Ions and the Influence of Reactants Ratio on the Products at Room Temperature

  • Youngjin Jeon
    • Journal of the Korean Chemical Society
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    • v.68 no.2
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    • pp.82-86
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    • 2024
  • This paper presents the solid-state synthesis of insoluble Prussian blue (Fe4[Fe(CN)6]3·xH2O, PB) in a ball mill, utilizing the fundamental components of PB. Solid-state synthesis offers several advantages, such as being solvent-free, quantitative, and easily scalable for industrial production. Traditionally, the solid-state synthesis of PB has been limited to the reaction between iron(II/III) ions and hexacyanoferrate(II/III) complex ions, essentially an extension of the solution-based coprecipitation method to solid-state reaction. Taking a bottom-up approach, a reaction is designed where the reactants consist of the basic building blocks of PB: Fe2+ ions and CN- ions. The reaction, with a molar ratio of Fe2+ and CN- corresponding to 1:2.8, yields PB, while a ratio of 1:6.6 results in a mixture of potassium hexacyanoferrate(II) (K4Fe(CN)6), potassium chloride (KCl), and potassium cyanide (KCN). This synthetic approach holds promise for environmentally friendly methods to synthesize multimetallic PB with maximum entropy in nearly quantitative yield.

A Study on the Synthesis of Acrylic Phenol Resins and Their Properties as a Paint (아크릴계 페놀수지 합성과 이를 이용한 도료의 물성연구)

  • Hwang, Sue In;Kim, Young Jin;Kim, Dong Kwon
    • Applied Chemistry for Engineering
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    • v.24 no.2
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    • pp.171-176
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    • 2013
  • The need of volatile organic compound (VOC) free coating material has been increased to solve environmental problems such as the global warming. Nowadays, about 70~80% of coating materials used in the worldwide are a liquid type. Therefore, the development of non-solvent coating material that can minimize VOCs emissions is necessary to solve the global warming problem. In this study, acrylic monomers were added to develop non-solvent paints in order to improve disadvantages of the poor adhesion of a conventional phenolic resin caused by acidification. As a result, the blend resins of 2.818 Mpa phenol- formaldehyde resin/poly methyl methacrylate (PE/PMMA) has the best properties and performances for the adhesives.

Synthesis of Long Chain Alkyl Urocanate and Solubilization in Organic Solvent (긴사슬 알킬 우로칸에스테르의 합성 및 유기물질에서의 가용성)

  • Ro, Y.C.;Jeong, H.K.;Nam, K.D.;Lee, J.H.
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.1
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    • pp.83-91
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    • 1993
  • The syntheses of urocanic acid esters was optimized, starting from p-toluenesulfonic acid salt of this acid and long chain fatty alcohols in the organic solvent and extracting water from it by means of azeotropic Compound. The salts of these urocanic acid esters showed amphoteric properties, but their micellization enhances their rate of hydrolysis leading to the free amine. Nevertheless the long chain gives to the esters themselves an amphoteric character allowing their solubilization in micellar media and in microemulsions the result, yield could enhanced.

Synthesis of Diacylglycerol-Enriched Functional Lipid Containing DHA by Lipase-Catalyzed in Solvent-Free System (비 용매계에서 DHA가 함유된 Diacylglycerol의 효소적 반응에 의한 합성연구)

  • Kim, Nam-Sook;Lee, Ki-Teak
    • Korean Journal of Food Science and Technology
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    • v.37 no.4
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    • pp.584-589
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    • 2005
  • Structured triacylglycerol (SL-TAG) was synthesized by enzymatic interesterification with algae oil and soybean oil in solvent-free system. Structured di- and monoacylglycerol (SL-DAG/MAG) were produced by glycerolysis with SL-TAG and glycerol catalyzed by lipase. Reactions were performed by sn-1.3 specific Lipozyme RM IM lipase from Rhizomucor miehei (interesterification, 11%; glycerolysis 5% by weight of total substrates) in solvent-free system using stirred-batch type reactor. SL-DAG/MAG contained TAG (42,3 area%), 1,3-DAG (19.2 area%), 1,2-DAG (22.2 area%), MAG (16.0 area%), and free fatty acid (0.2 area%). Iodine and saponification values of SL-DAG/MAG were 208.8 and 179.6, respectively. SL-DAG/MAG appeared yellowish in color.

Synthesis and Characterization of Poly(urethane-ethyl acrylate) Hybrid Emulsion (폴리(우레탄-에틸 아크릴레이트) 혼성 에멀젼의 합성과 물성 비교 연구)

  • Cheong, In Woo;Lee, Jong Kil;Kim, Jung Hyun
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.86-92
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    • 2005
  • Poly(urethaneethyl acrylate) hybrid emulsions were synthesized to improve their thermomechanical and solvent resistance properties. In the synthesis, dimethylol propionic acid was used to impart hydrophilicity to the hybrid polymers, and ethyl acrylate monomer was added to the polyurethane prepolymer after neutralization with triethylamine. After dispersion of the neutralized prepolymer, chain extension was carried out with ethylene diamine. Consequently, poly(urethaneethyl acrylate) hybrid emulsion was prepared via soap free emulsion polymerization of ethyl acrylate with reduction-oxidation initiator couple of t-butyl hydroperoxide/sodium bisulfite at $50^{\circ}C$. Tehsile strength, 100% modulus, elongation, and solvent-resistance properties of the hybrid emulsion were measured and compared with those of polyurethane homopolymer, poly(ethyl acrylate) homopolymer, and simple blended samples.

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.

Alum Catalyzed Convenient Synthesis of Quino[2,3-b][1,5 benzoxazepine α-Aminophosphonate Derivatives

  • Sonar, Swapnil S.;Sadaphal, Sandip A.;Shitole, Nana V.;Jogdand, Nivrutti R.;Shingate, Bapurao B.;Shingare, Murlidhar S.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.8
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    • pp.1711-1714
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    • 2009
  • We have described an efficient synthesis of quino[2,3-b][1,5]benzoxazepine α-aminophosphonate derivatives by the nucleophilic addition of triethyl phosphite to substituted quino[2,3-b][1,5]benzoxazepines promoted by easily available, inexpensive and mild catalyst KAl(S$O_4)_2{\cdot}12H_2$O(alum). The reactions proceed smoothly at room temperature under solvent-free reaction conditions and providing high yield of product in very short reaction time.

Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones Using HClO4-SiO2 as a Heterogeneous and Recyclable Catalyst

  • Maheswara, Muchchintala;Oh, Sang-Hyun;Kim, Ke-Tack;Do, Jung-Yun
    • Bulletin of the Korean Chemical Society
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    • v.29 no.9
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    • pp.1752-1754
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    • 2008
  • A simple and efficient synthesis of 3,4-dihydropyrimidinones or thiones is described, using silica-supported perchloric acid ($HClO_4-SiO_2$) as a heterogeneous catalyst from an aldehyde, $\beta$-dicarbonyl compound, and urea or thiourea under solvent-free conditions. Compared to the classical Biginelli reactions, this method consistently has the advantage of high yields, short reaction time, easy separation, and tolerance towards various functional groups.