WorldWideScience

Sample records for catalyzed solvent-free one-pot

  1. Nanocrystalline copper(II oxide-catalyzed one-pot four- component synthesis of polyhydroquinoline derivativesunder solvent-free conditions

    Directory of Open Access Journals (Sweden)

    J. Safaei-Ghomi

    2011-07-01

    Full Text Available The efficient and environmentally friendly method for the one-pot synthesis of polyhydroquinolines has been developed in the presence of CuO nanoparticles. The multi-component reactions of aldehydes, dimedone, ethyl acetoacetate andammonium acetate were carried out under solvent-free conditions to afford some polyhydroquinoline derivatives. This method provides several advantages including high yields, low reaction times and little catalyst loading.

  2. One-pot Solvent-free Catalytic Dimerization Reaction of ...

    Indian Academy of Sciences (India)

    Abstract. In this study, we report a smooth one-pot, solvent-free catalytic dimerization of phenylacetylene. (1) to 1-phenylnaphthalene (2) by Cu/C at room temperature in good yield (∼100%). In the computational study, the structure of the 1-phenylnaphthalene was optimized by DFT-B3LYP/6-31G* method. The rotation.

  3. Gypsum-Catalyzed One-Pot Synthesis of 3,4-Dihydropyrimidin-2(1H Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Taoues Boumoud

    2011-01-01

    Full Text Available In view of the emerging importance of the green chemistry principles in chemical and pharmaceutical industries, we disclose, herein, a new economic approach producing the biologically active dihydropyrimidinones in good yields using the solventless one-pot Biginelli condensation in the presence of gypsum as an environmental friendly and recycled catalyst.

  4. Microwave Assisted Convenient One-Pot Synthesis of Coumarin Derivatives via Pechmann Condensation Catalyzed by FeF3 under Solvent-Free Conditions and Antimicrobial Activities of the Products

    Directory of Open Access Journals (Sweden)

    Vahid Vahabi

    2014-08-01

    Full Text Available A rapid and efficient solvent-free one-pot synthesis of coumarin derivatives by Pechmann condensation reactions of phenols with ethyl acetoacetate using FeF3 as a catalyst under microwave irradiation is described. This one-pot synthesis on a solid inorganic support provides the products in good yields. The newly synthesized compounds were systematically characterized by IR, 1H-NMR, 13C-NMR, MS and elemental CHN analyses. The proposed solvent-free microwave irradiation method using the environmentally friendly catalyst FeF3 offers the unique advantages of high yields, shorter reaction times, easy and quick isolation of the products, excellent chemoselectivity, and a one-pot, green synthesis. The products were screened for antimicrobial activity, and the results showed that the compounds reacted against all the tested bacteria.

  5. Multicomponent One-Pot Synthesis of Substituted Hantzsch Thiazole Derivatives Under Solvent Free Conditions

    Directory of Open Access Journals (Sweden)

    Bhaskar S. Dawane

    2009-01-01

    Full Text Available Thiazole derivatives were prepared by one-pot procedure by the reaction of α-haloketones, thiourea and substituted o-hydroxybenzaldehyde under environmentally solvent free conditions.

  6. A Facile One-Pot Solvent-Free Synthesis of 1,2-Dihydro-1-arylnaphtho[1,2-e][1,3]oxazine-3-ones Catalyzed by Wet Cyanuric Chloride

    Directory of Open Access Journals (Sweden)

    Firouzeh Nemati

    2013-01-01

    Full Text Available A novel one-pot synthesis of 1,2-dihydro-1-arylnaphtho[1,2-e][1,3]oxazine-3-ones by condensation of a variety of aldehydes with β-naphthol and urea or thiourea in the presence of wet cyanuric chloride under solvent-free condition has been described. High yields, simple procedure, easy workup, short reaction times, and avoiding the use of organic solvent are the advantages of this green methodology.

  7. Nano crystalline ZnO catalyzed one pot three-component synthesis of 7-alkyl-6H,7H- naphtho[1',2':5,6]pyrano[3,2-c] chromen-6-ones under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    M. J. Piltan

    2016-08-01

    Full Text Available In the present paper, an efficient one-pot synthesis of 7-alkyl-6H,7H-naphtho[1',2':5,6]pyrano[3,2-c]chromen-6-ones is described by three-component reaction of β-naphthol, aromatic aldehydes and 4-hydroxycoumarin using ZnO nanoparticles under solvent-free conditions. The present method provides a novel and efficient procedure for the synthesis of chromene derivatives with some advantageous such as short reaction times, easy workup, high yields, wide range of products, reusability of the catalyst, little catalyst loading and green conditions in the presence of ZnO nanoparticles (7 mol% at 110 ºC.

  8. Solvent free one pot synthesis of amidoalkyl naphthols over phosphotungstic acid

    Directory of Open Access Journals (Sweden)

    Divya P. Narayanan

    2017-07-01

    Full Text Available Montmorillonite KSF clay was effectively modified by the encapsulation of phosphotungstic acid into the clay layers via sonication followed by incipient wet impregnation method. The prepared catalysts were characterized by X-ray diffraction (XRD, Fourier-transform infrared spectroscopy (FTIR and scanning electron microscopy (SEM techniques. The catalytic activities of the prepared systems were investigated in the solvent free synthesis of amidoalkyl naphthols by the multicomponent one-pot condensation of an aldehyde, β-naphthol and an amide or urea. Excellent yield, shorter reaction time, easy work-up, and reusability of the catalyst are the main attractions of this green procedure.

  9. Mesoporous molecular sieve MCM-41 catalyzed one-pot synthesis of 3,4-dihydro-2(1H-pyrimidinones and –thiones under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Rahim Hekmatshoar

    2011-08-01

    Full Text Available An efficient synthesis of 3,4-dihydro-2(1H-pyrimidinones and -thiones using MCM-41 as the catalyst from an aldehyde, β-keto ester, and urea or thiourea under solvent-free conditions is described.

  10. Mesoporous molecular sieve MCM-41 catalyzed one-pot synthesis ...

    African Journals Online (AJOL)

    An efficient synthesis of 3,4-dihydro-2(1H)-pyrimidinones and -thiones using MCM-41 as the catalyst from an aldehyde, β-keto ester, and urea or thiourea under solvent-free conditions is described. KEY WORDS: Biginelli reaction, Dihydropyrimidinones, MCM-41, One-pot, Reusable. Bull. Chem. Soc. Ethiop. 2011, 25(2) ...

  11. Facile solvent-free one-pot synthesis of pyranobenzopyrans and ...

    Indian Academy of Sciences (India)

    The condensation of hydroxyl coumarins in a facile one-pot procedure with active methylene esters to afford novel benzopyrans under solventless conditions is described. The products underwent further condensation and cyclization reactions to form novel heterocycles.

  12. One-pot solvent-free rapid and green synthesis of 3,4-dihydropyrano[c]chromenes using grindstone chemistry

    Directory of Open Access Journals (Sweden)

    Devji S. Patel

    2016-09-01

    Full Text Available An easy solvent-free method is described for the synthesis of 3,4-dihydropyrano[c]chromenes by a one pot three component coupling reaction of aromatic aldehydes, malononitrile, and 4-hydroxycoumarin using basic ionic liquid as the catalyst by grindstone chemistry. The salient features of this one pot protocol are short reaction times, cleaner reaction profiles and simple workup.

  13. NANO CRYSTALLINE ZnO CATALYZED ONE POT THREE ...

    African Journals Online (AJOL)

    naphtho[1',2':5,6]pyrano[3,2- c]chromen-6-ones is described by three-component reaction of β-naphthol, aromatic aldehydes and 4- hydroxycoumarin using ZnO nanoparticles under solvent-free conditions. The present method provides a ...

  14. A Simple, Rapid and Mild One Pot Synthesis of Benzene Ring Acylated and Demethylated Analogues of Harmine under Solvent-free Conditions

    Directory of Open Access Journals (Sweden)

    Bina S. Siddiqui

    2008-08-01

    Full Text Available A simple, rapid, solvent-free, room temperature one pot synthesis of benzene ring acylated and demethylated analogues of harmine using acyl halides/acid anhydrides and AlCl3 has been developed. Eight different acyl halides/acid anhydrides were used in the synthesis. The resulting mixture of products was separated by column chromatography to afford 10- and 12-monoacyl analogues, along with 10,12-diacyl-11-hydroxy products. In five cases the corresponding 10-acyl-11-hydroxy analogues were also obtained. Yields from the eight syntheses (29 products in total were in the 6-34% range and all compounds were fully characterized.

  15. Solvent free lipase catalyzed synthesis of butyl caprylate

    Indian Academy of Sciences (India)

    MEERA T SOSE

    2017-11-10

    Nov 10, 2017 ... Special Issue on Recent Trends in the Design and Development of Catalysts and their Applications. Solvent free lipase catalyzed synthesis of butyl caprylate. MEERA T SOSE, SNEHA R .... and keeping others constant. It is also very important to prevent excess water formation as it results to give back the ...

  16. Orthogonal protection of saccharide polyols through solvent-free one-pot sequences based on regioselective silylations

    Directory of Open Access Journals (Sweden)

    Serena Traboni

    2016-12-01

    Full Text Available tert-Butyldimethylsilyl (TBDMS and tert-butyldiphenylsilyl (TBDPS are alcohol protecting groups widely employed in organic synthesis in view of their compatibility with a wide range of conditions. Their regioselective installation on polyols generally requires lengthy reactions and the use of high boiling solvents. In the first part of this paper we demonstrate that regioselective silylation of sugar polyols can be conducted in short times with the requisite silyl chloride and a very limited excess of pyridine (2–3 equivalents. Under these conditions, that can be regarded as solvent-free conditions in view of the insolubility of the polyol substrates, the reactions are faster than in most examples reported in the literature, and can even be further accelerated with a catalytic amount of tetrabutylammonium bromide (TBAB. The strategy proved also useful for either the selective TBDMS protection of secondary alcohols or the fast per-O-trimethylsilylation of saccharide polyols. In the second part of the paper the scope of the silylation approach was significantly extended with the development of unprecedented “one-pot” and “solvent-free” sequences allowing the regioselective silylation/alkylation (or the reverse sequence of saccharide polyols in short times. The developed methodologies represent a very useful and experimentally simple tool for the straightforward access to saccharide building-blocks useful in organic synthesis.

  17. Orthogonal protection of saccharide polyols through solvent-free one-pot sequences based on regioselective silylations

    Science.gov (United States)

    Traboni, Serena; Bedini, Emiliano

    2016-01-01

    tert-Butyldimethylsilyl (TBDMS) and tert-butyldiphenylsilyl (TBDPS) are alcohol protecting groups widely employed in organic synthesis in view of their compatibility with a wide range of conditions. Their regioselective installation on polyols generally requires lengthy reactions and the use of high boiling solvents. In the first part of this paper we demonstrate that regioselective silylation of sugar polyols can be conducted in short times with the requisite silyl chloride and a very limited excess of pyridine (2–3 equivalents). Under these conditions, that can be regarded as solvent-free conditions in view of the insolubility of the polyol substrates, the reactions are faster than in most examples reported in the literature, and can even be further accelerated with a catalytic amount of tetrabutylammonium bromide (TBAB). The strategy proved also useful for either the selective TBDMS protection of secondary alcohols or the fast per-O-trimethylsilylation of saccharide polyols. In the second part of the paper the scope of the silylation approach was significantly extended with the development of unprecedented “one-pot” and “solvent-free” sequences allowing the regioselective silylation/alkylation (or the reverse sequence) of saccharide polyols in short times. The developed methodologies represent a very useful and experimentally simple tool for the straightforward access to saccharide building-blocks useful in organic synthesis. PMID:28144345

  18. Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Sudipta Pathak

    2013-11-01

    Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

  19. p -Dimethylaminopyridine (DMAP: A highly efficient catalyst for one pot, solvent free synthesis of substituted 2-amino-2-chromenes under microwave irradiation

    Directory of Open Access Journals (Sweden)

    Kamlesh R. Desale

    2012-01-01

    Full Text Available A highly efficient, green and expeditious method is described for the synthesis of substituted 2-amino-2-chromenes employing one pot three component condensation of aromatic aldehydes, malononitrile and activated phenol in presence of p-dimethylaminopyridine (10 mol % as a catalyst under microwave irradiation. The present method is operationally simple and offers many advantages such as high yield, short reaction time and simple workup.

  20. Poly(4-vinylpyridine efficiently catalyzed one-pot four-component synthesis of pyrano[2,3-c]pyrazoles

    Directory of Open Access Journals (Sweden)

    Jalal Albadi

    2014-10-01

    Full Text Available An efficient one-pot synthesis of pyrano[2,3-c]pyrazoles via four-component reaction of phenyl hydrazine, ethyl acetoacetate, malononitrile and aromatic aldehydes, catalyzed by poly(4-vinylpyridine is reported. This method provides many advantages such as, atom-economy, easy work up, clean procedure, short reaction times and high yields of products.

  1. Highly efficient one-pot three-component synthesis of naphthopyran derivatives in water catalyzed by hydroxyapatite

    Science.gov (United States)

    An expeditious and efficient protocol for the synthesis of naphthopyrans has been developed that proceeds via one-pot three-component sequential reaction in water catalyzed by hydroxyapatite or sodium-modified-hydroxyapatite. The title compounds have been obtained in high yield a...

  2. A novel one-pot synthesis of spirooxindole derivatives catalyzed by ...

    African Journals Online (AJOL)

    Nano zinc oxide was explored as a heterogeneous and reusable catalyst for the one-pot synthesis of spirooxindoles via three-component reaction between urea, isatin, and 1,3-dicarbonyl compounds. KEY WORDS: Nano-ZnO, Spirooxindoles, Isatin. Bull. Chem. Soc. Ethiop. 2013, 27(2), 309-314.

  3. Yb(OTf){sub 3}-catalyzed one-pot three component synthesis for tertiary amines

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Bum Seok; Kim, Ji Hye; Nam, Tae Kyu; Jang, Doo Ok [Dept. of Chemistry, Yonsei University, Wonju (Korea, Republic of)

    2015-07-15

    Tertiary amine functionality is found in many natural bioactive products such as alkaloids, amino acids, nucleic acids, pharmaceuticals, and agrochemicals. Tertiary amines have also been used as building blocks for nitrogen-containing organic compounds and synthetic polymers. A one-pot method for direct reductive amination of aldehydes has been developed to synthesize tertiary amines using HMDS as a nitrogen source in the presence of Yb(OTf ){sub 3}. With a stoichiometric amount of HMDS, the reaction afforded the desired tertiary amines without competitive reduction of the parent carbonyl compounds. This reaction offers a convenient and efficient protocol for synthesizing aromatic and aliphatic tertiary amines under mild reaction conditions.

  4. Sequential Dy(OTf)3 -Catalyzed Solvent-Free Per-O-Acetylation and Regioselective Anomeric De-O-Acetylation of Carbohydrates.

    Science.gov (United States)

    Yan, Yi-Ling; Guo, Jiun-Rung; Liang, Chien-Fu

    2017-09-19

    Dysprosium(III) trifluoromethanesulfonate-catalyzed per-O-acetylation and regioselective anomeric de-O-acetylation of carbohydrates can be tuned by adjusting the reaction medium. In this study, the per-O-acetylation of unprotected sugars by using a near-stoichiometric amount of acetic anhydride under solvent-free conditions resulted in the exclusive formation of acetylated saccharides as anomeric mixtures, whereas anomeric de-O-acetylation in methanol resulted in a moderate-to-excellent yield. Reactions with various unprotected monosaccharides or disaccharides followed by a semi-one-pot sequential conversion into the corresponding acetylated glycosyl hemiacetal also resulted in high yields. Furthermore, the obtained hemiacetals could be successfully transformed into trichloroimidates after Dy(OTf) 3 -catalyzed glycosylation. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Transglutaminase-Catalyzed Bioconjugation Using One-Pot Metal-Free Bioorthogonal Chemistry.

    Science.gov (United States)

    Rachel, Natalie M; Toulouse, Jacynthe L; Pelletier, Joelle N

    2017-10-18

    General approaches for controlled protein modification are increasingly sought-after in the arena of chemical biology. Here, using bioorthogonal reactions, we present combinatorial chemoenzymatic strategies to effectuate protein labeling. A total of three metal-free conjugations were simultaneously or sequentially incorporated in a one-pot format with microbial transglutaminase (MTG) to effectuate protein labeling. MTG offers the particularity of conjugating residues within a protein sequence rather than at its extremities, providing a route to labeling the native protein. The reactions are rapid and circumvent the incompatibility posed by metal catalysts. We identify the tetrazine ligation as most-reactive for this purpose, as demonstrated by the fluorescent labeling of two proteins. The Staudinger ligation and strain-promoted azide-alkyne cycloaddition are alternatives. Owing to the breadth of labels that MTG can use as a substrate, our results demonstrate the versatility of this system, with the researcher being able to combine specific protein substrates with a variety of labels.

  6. L-proline-catalyzed enantioselective one-pot cross-Mannich reaction of aldehydes.

    Science.gov (United States)

    Hayashi, Yujiro; Urushima, Tatsuya; Tsuboi, Wataru; Shoji, Mitsuru

    2007-01-01

    This protocol describes a procedure for the synthesis of syn-beta-amino alpha-substituted aldehydes, versatile intermediates in synthetic organic chemistry, via asymmetric, direct, one-pot, three-component, cross-Mannich reaction of two different aldehydes. The reaction consists of two steps; one is the formation of imine by the reaction of aldehyde and p-anisidine in the presence of Pro, and the second step is the enantioselective addition reaction of enamine generated from the other aldehyde and Pro with the imine generated in the first step. As the aldehyde easily racemizes, gamma-amino alcohol was isolated and characterized after reduction. The yield and diastereo- and enantioselectivities are generally excellent. It will take approximately 26 h to complete the protocol: 0.5 h to set up the reaction, 20.5 h for the reaction and 5 h for the isolation and purification.

  7. Copper-catalyzed one-pot synthesis of N-aryl oxazolidinones from amino alcohol carbamates.

    Science.gov (United States)

    Mahy, William; Plucinski, Pawel K; Frost, Christopher G

    2014-10-03

    An efficient sequential intramolecular cyclization of amino alcohol carbamates followed by Cu-catalyzed cross-coupling with aryl iodides under mild conditions has been developed. The reaction occurred in good yields and tolerated aryl iodides containing functionalities such as nitriles, ketones, ethers, and halogens. Heteroaryl iodides and substituted amino alcohol carbamates were also well tolerated.

  8. Solvent-free Al(OTf)3-catalyzed aminolysis of 1,2-epoxides by 2-picolylamine: a key step in the synthesis of ionic liquids.

    Science.gov (United States)

    Fringuelli, Francesco; Pizzo, Ferdinando; Tortoioli, Simone; Vaccaro, Luigi

    2004-10-29

    Beta-Amino alcohols N-2'-pyridylmethyl substituted 3 have been prepared in excellent yields under mild conditions by the first Lewis acid-catalyzed aminolysis of 1,2-epoxides 1 with the bihaptic amine 2-picolylamine (2) with use of 5 mol % of Al(OTf)(3) under solvent-free conditions. As a representative of a new class of ionic liquids, cis-5-[(4'-methylphenyl)sulfonyl]-1,2,3,4,4a,5,6,11a-octahydropyrido[1,2-a]quinoxalin-11-ium methanesulfonate (6) and its chloride derivative 7 have been synthesized under environmentally friendly conditions by the one-pot aminolysis of cyclohexene oxide (1a) with 2 and intramolecular cyclization of the resulting 2-[(pyridin-2'-yl)methylamino]cyclohexanol (3a).

  9. Polycyclization Enabled by Relay Catalysis: One-Pot Manganese-Catalyzed C-H Allylation and Silver-Catalyzed Povarov Reaction.

    Science.gov (United States)

    Chen, Shi-Yong; Li, Qingjiang; Liu, Xu-Ge; Wu, Jia-Qiang; Zhang, Shang-Shi; Wang, Honggen

    2017-06-09

    In this study, a Mn I /Ag I -based relay catalysis process is described for the one-pot synthesis of polycyclic products by a formal [3+2] and [4+2] cycloaddition reaction cascade. A manganese(I) complex catalyzed the first example of directed C-H allylation with allenes, setting the stage for an in situ Povarov cyclization catalyzed by silver(I). The reaction proceeds with high bond-forming efficiency (three C-C bonds), broad substrate scope, high regio- and stereoselectivity, and 100 % atom economy. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Ultrasound assisted lipase catalyzed synthesis of cinnamyl acetate via transesterification reaction in a solvent free medium.

    Science.gov (United States)

    Tomke, Prerana D; Rathod, Virendra K

    2015-11-01

    Cinnamyl acetate is known for its use as flavor and fragrance material in different industries such as food, pharmaceutical, cosmetic etc. This work focuses on ultrasound assisted lipase (Novozym 435) catalyzed synthesis of cinnamyl acetate via transesterification of cinnamyl alcohol and vinyl acetate in non-aqueous, solvent free system. Optimization of various parameters shows that a higher yield of 99.99% can be obtained at cinnamyl alcohol to vinyl acetate ratio of 1:2 with 0.2% of catalyst, at 40°C and 150 rpm, with lower ultrasound power input of 50 W (Ultrasound intensity 0.81 W/cm(2)), at 25 kHz frequency, 50% duty cycle. Further, the time required for the maximum conversion is reduced to 20 min as compared to 60 min of conventional process. Similarly, the enzyme can be successfully reused seven times without loss of enzyme activity. Thus, ultrasound helps to enhance the enzyme catalyzed synthesis of flavors. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Nafion®-catalyzed microwave-assisted Ritter reaction: An atom-economic solvent-free synthesis of amides

    Science.gov (United States)

    An atom-economic solvent-free synthesis of amides by the Ritter reaction of alcohols and nitriles under microwave irradiation is reported. This green protocol is catalyzed by solid supported Nafion®NR50 with improved efficiency and reduced waste production.

  12. Microwave Assisted Expeditious and Green Cu(II-Clay Catalyzed Domino One-Pot Three Component Synthesis of 2H-indazoles

    Directory of Open Access Journals (Sweden)

    Bashir Ahmad Dar

    2018-01-01

    How to Cite: Dar, B.A., Safvi, S.W., Rizvi, M.A. (2018. Microwave Assisted Expeditious and Green Cu(II-Clay Catalyzed Domino One-Pot Three Component Synthesis of 2H-indazoles. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (1: 82-88 (doi:10.9767/bcrec.13.1.963.82-88

  13. Synthesis of 2-aryl-2H-benzotrizoles from azobenzenes and N-sulfonyl azides through sequential rhodium-catalyzed amidation and oxidation in one pot.

    Science.gov (United States)

    Ryu, Taekyu; Min, Jiae; Choi, Wonseok; Jeon, Woo Hyung; Lee, Phil Ho

    2014-06-06

    An efficient synthetic method of 2-aryl-2H-benzotriazoles from nonprefunctionalized azobenzenes and N-sulfonyl azides via sequential Rh-catalyzed amidation (C-N bond formation) and oxidation (N-N bond formation) with PhI(OAc)2 in one pot is reported.

  14. Cyanuric Chloride-Catalyzed Michael Addition of Indoles to Nitroolefins under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Xiao Juan Yang

    2013-01-01

    Full Text Available Cyanuric chloride is an inexpensive, efficient, and mild catalyst for the Michael addition of indoles to nitroolefins at 70°C under solvent-free conditions. The simple experimental procedure, solvent-free reaction conditions, utilization of an inexpensive and readily available catalyst, short period of conversion, and excellent yields are the advantages of the present method.

  15. One-Pot Synthesis of Novel Chiral β-Amino Acid Derivatives by Enantioselective Mannich Reactions Catalyzed by Squaramide Cinchona Alkaloids

    Directory of Open Access Journals (Sweden)

    Kankan Zhang

    2013-05-01

    Full Text Available An efficient one-pot synthesis of novel β-amino acid derivatives containing a thiadiazole moiety was developed using a chiral squaramide cinchona alkaloid as organocatalyst. The reactions afforded chiral β-amino acid derivatives in moderate yields and with moderate to excellent enantioselectivities. The present study demonstrated for the first time the use of a Mannich reaction catalyzed by a chiral bifunctional organocatalyst for the one-pot synthesis of novel β-amino acid derivatives bearing a 1,3,4-thiadiazole moiety on nitrogen.

  16. Mechanochemical Solvent-Free and Catalyst-Free One-Pot Synthesis of Pyrano[2,3-d]Pyrimidine-2,4(1H,3H-Diones with Quantitative Yields

    Directory of Open Access Journals (Sweden)

    M. Reza Naimi-Jamal

    2009-01-01

    Full Text Available Solvent-free synthesis of pyrano[2,3-d]pyrimidine-2,4(1H,3H-diones by ball-milling and without any catalyst is described. This method provides several advantages such as being environmentally friendly, using a simple workup procedure, and affording high yields.

  17. E-Factor minimized hydrophosphonylation of aldehydes catalyzed by polystyryl-BEMP under solvent-free conditions.

    Science.gov (United States)

    Angelini, Tommaso; Bonollo, Simona; Lanari, Daniela; Pizzo, Ferdinando; Vaccaro, Luigi

    2013-08-14

    An efficient protocol for the hydrophosphonylation of aromatic and aliphatic aldehydes catalyzed by PS-BEMP under solvent-free conditions (SolFC) has been reported. Addition reactions were performed by using equimolar amounts of reagents and the resulting α-hydroxyphosphonates were isolated with simple workup procedures. A large scale protocol for the preparation of a representative α-hydroxyphosphonate 3a has been also set up using a flow reactor.

  18. β-cyclodextrin-polyurethane polymer: A neutral and eco-friendly heterogeneous catalyst for the one-pot synthesis of 1,4-dihydropyridine and polyhydroquinolien derivatives via Hantzsch reaction under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Kiasat Ali Reza

    2014-01-01

    Full Text Available An efficient synthesis of 1,4-dihydropyridine & polyhydroquinolien derivatives using b-Cyclodextrin-polyurethane polymer (β-CDPU as a stationary microvessel and neutral heterogeneous catalyst via a four component coupling of aldehydes, β-ketoester (2 mol and ammonium acetate under solvent-free conditions is described. Compared with the classical Hantzsch reaction, this new method has the advantages of good yield, short reaction time and methodological simplicity. β-CDPU was proved to be an efficient heterogeneous catalyst which could be easily handled and removed from the reaction mixture by simple filtration, and also recovered and reused without loss of reactivity.

  19. Carbon-based Solid Acid Catalyzed One-pot Mannich Reaction: A Facile Synthesis of β-Amino Carbonyl Compounds

    Energy Technology Data Exchange (ETDEWEB)

    Davoodnia, Abolghasem; Tavakoli-Nishaburi, Afsaneh; Tavakoli-Hoseini, Niloofar [Islamic Azad University, Mashhad (Iran, Islamic Republic of)

    2011-02-15

    A simple and efficient method for the synthesis of β-amino carbonyl compounds by one-pot three-component Mannich reaction of acetophenone, aromatic aldehydes and aromatic amines using a carbon-based solid acid (CBSA), as an effective and reusable catalyst, is described. The present methodology offers several advantages such as simple procedure with an easy work-up, shorter reaction times, and high yields.

  20. Metallocene catalyzed synthesis of fungistatic vicinal aminoalcohols under solvent free conditions.

    Science.gov (United States)

    Mancilla, Gabriela; Durán-Patrón, Rosa M; Macías-Sánchez, Antonio J; Collado, Isidro G

    2010-11-15

    Group 4 and 5 metallocenes, Cp(2)TiCl(2), Cp(2)ZrCl(2) and Cp(2)VCl(2), have been evaluated as catalyst in the solvent free, room temperature, preparation of vicinal aminoalcohols. The regioselectivity of the reaction and the fungistatic activity of the prepared compounds against Botrytis cinerea and Colletotrichum gloeosporioides are discussed. Copyright © 2010 Elsevier Ltd. All rights reserved.

  1. Sequential One-Pot Ruthenium-Catalyzed Azide−Alkyne Cycloaddition from Primary Alkyl Halides and Sodium Azide

    KAUST Repository

    Johansson, Johan R.

    2011-04-01

    An experimentally simple sequential one-pot RuAAC reaction, affording 1,5-disubstituted 1H-1,2,3-triazoles in good to excellent yields starting from an alkyl halide, sodium azide, and an alkyne, is reported. The organic azide is formed in situ by treating the primary alkyl halide with sodium azide in DMA under microwave heating. Subsequent addition of [RuClCp*(PPh 3) 2] and the alkyne yielded the desired cycloaddition product after further microwave irradiation. © 2011 American Chemical Society.

  2. Indium(III)-catalyzed synthesis of N-substituted pyrroles under solvent-free conditions

    OpenAIRE

    Chen, Jiu-Xi; Liu, Miao-Chang; Yang, Xiao-Liang; Ding, Jin-Chang; Wu, Hua-Yue

    2008-01-01

    A variety of N-substituted pyrroles have been synthesized by reacting γ-diketones (R¹C(O)CH2CH2C(O)R²: R¹, R² = Me, Ph) with amines (RNH2: R=Alkyl, Aryl, TsNH) or diamines (1,6-diaminohexane and 1,2-diaminoethane) in the presence of indium tribromide, indium trichloride or indium trifluoromethanesulfonate at room temperature under solvent-free conditions. The experiment protocol features simple operations, and the products are isolated in high to excellent yields (81-98%). Vários pirróis N...

  3. One-Pot Lipase-Catalyzed Enantioselective Synthesis of (R-(−-N-Benzyl-3-(benzylaminobutanamide: The Effect of Solvent Polarity on Enantioselectivity

    Directory of Open Access Journals (Sweden)

    Marina A. Ortega-Rojas

    2017-12-01

    Full Text Available The use of the solvent engineering has been applied for controlling the resolution of lipase-catalyzed synthesis of β-aminoacids via Michael addition reactions. The strategy consisted of the thermodynamic control of products at equilibrium using the lipase CalB as a catalyst. The enzymatic chemo- and enantioselective synthesis of (R-(−-N-benzyl-3-(benzylaminobutanamide is reported, showing the influence of the solvent on the chemoselectivity of the aza-Michael addition and the subsequent kinetic resolution of the Michael adduct; both processes are catalyzed by CalB and both are influenced by the nature of the solvent medium. This approach allowed us to propose a novel one-pot strategy for the enzymatic synthesis of enantiomerically enriched β-aminoesters and β-aminoacids.

  4. Cinnamyl acetate synthesis by lipase-catalyzed transesterification in a solvent-free system.

    Science.gov (United States)

    Geng, Bo; Wang, Mengfan; Qi, Wei; Su, Rongxin; He, Zhimin

    2012-01-01

    Cinnamyl acetate was synthesized using immobilized lipase through transesterification between ethyl acetate and cinnamyl alcohol. In the solvent-free system, ethyl acetate acted as not only the acyl donor but also as the solvent of cinnamyl alcohol. Conversion (90.06%) was achieved after 3 H when transesterification was carried out at ethyl acetate/cinnamyl alcohol 15:1, 2.67 g L of lipase (Novozym 435) loading, and 40°C. Excellent stability and reusability of the enzyme resulted from the moderate reaction system. Kinetic studies showed that the Michaelis constants for ethyl acetate and cinnamyl alcohol and the inhibition constant of cinnamyl alcohol were 2.241, 206.82, and 0.461 mmol L⁻¹, respectively, which indicated that the reaction complied with the Ping-Pong Bi-Bi mechanism, with the inhibition of cinnamyl alcohol on lipase. Copyright © 2012 International Union of Biochemistry and Molecular Biology, Inc.

  5. Ultrasound promoted facile one pot synthesis of triazole derivatives catalyzed by functionalized graphene oxide Cu(I) complex under mild conditions.

    Science.gov (United States)

    Naeimi, Hossein; Shaabani, Rahele

    2017-01-01

    A facile one pot three component reaction of alkyl halides, sodium azide with terminal alkynes can be catalyzed by functionalized graphene oxide copper (I) complex under ultrasonic irradiation at room temperature. In this protocol, the 1,4-disubstituted 1,2,3-triazoles were afforded as target pure products in excellent yields and short reaction times. The prepared catalyst has been characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction spectroscopy (XRD), Energy Dispersive X-ray (EDX) and field emission scanning electron microscopy (FE-SEM) techniques. Also, the catalyst is chemoselective and stable and can be reused several times without any appreciable loss of its catalytic activity. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Lipophilic (hydroxy)phenylacetates by solvent-free lipase-catalyzed esterification and transesterification in vacuo.

    Science.gov (United States)

    Weitkamp, Petra; Weber, Nikolaus; Vosmann, Klaus

    2008-07-09

    Various long-chain alkyl (hydroxy)phenylacetates were prepared in high yield by lipase-catalyzed transesterification of the corresponding short-chain alkyl hydroxyphenylacetates and fatty alcohols in equimolar ratios. The reactions were performed in vacuo at moderate temperatures in the absence of solvents and drying agents in direct contact with the reaction mixture. Immobilized lipase B from Candida antarctica (Novozym 435) was the most effective biocatalyst for the various transesterification reactions. Generally, Novozym 435-catalyzed transesterifications of short-chain alkyl (hydroxy)phenylacetates with long-chain alcohols led to higher conversions and enzyme activities than the corresponding esterifications. For example, the transesterification activity was up to 4-fold higher than the esterification activity for the formation of oleyl 4-hydroxy-3-methoxyphenylacetate using Novozym 435 as a biocatalyst. The relative transesterification activities were as follows: phenylacetate > 3-methoxyphenylacetate approximately 4-methoxyphenylacetate > 4-hydroxy-3-methoxyphenylacetate > 3-hydroxyphenylacetate approximately 4-hydroxyphenylacetate > 2-methoxyphenylacetate > 3,4-dihydroxyphenylacetate. With respect to the position of methoxy and hydroxy substituents, the transesterification activity of Novozym 435 decreased in the order meta approximately para > ortho. Compounds with inverse chemical structures, for example, tyrosyl oleate, were obtained by Novozym 435-catalyzed esterification and transesterification of fatty acids and their methyl esters, respectively, with 2-phenylethan-1-ols. In contrast to the transesterifications of short-chain alkyl (hydroxy)phenylacetates with fatty alcohols, higher conversions and enzyme activities were observed for the Novozym 435-catalyzed esterifications of (hydroxy)phenylethanols with long-chain fatty acids than the corresponding transesterifications with fatty acid methyl esters.

  7. One-pot Solvent-free Catalytic Dimerization Reaction of ...

    Indian Academy of Sciences (India)

    : 67149-67346, Kermanshah, Iran; Medical Biology Research Center, Kermanshah University of Medical Sciences, Kermanshah, Iran; Chemistry Department, Science Faculty, Islamic Azad University, Arak Branch, P.O. Box 38135-567, Arak, ...

  8. Highly efficient preparation of lipophilic hydroxycinnamates by solvent-free lipase-catalyzed transesterification.

    Science.gov (United States)

    Weitkamp, Petra; Vosmann, Klaus; Weber, Nikolaus

    2006-09-20

    Various medium- or long-chain alkyl cinnamates and hydroxycinnamates, including oleyl p-coumarate as well as palmityl and oleyl ferulates, were prepared in high yield by lipase-catalyzed transesterification of an equimolar mixture of a short-chain alkyl cinnamate and a fatty alcohol such as lauryl, palmityl, and oleyl alcohol under partial vacuum at moderate temperature in the absence of solvents and drying agents in direct contact with the reaction mixture. Immobilized lipase B from Candida antarctica was the most effective biocatalyst for the various transesterification reactions. Transesterification activity of this enzyme was up to 56-fold higher than esterification activity for the preparation of medium- and long-chain alkyl ferulates. The relative transesterification activities found for C. antarctica lipase were of the following order: hydrocinnamate > cinnamate > 4-hydroxyhydrocinnamate > 3-methoxycinnamate > 2-methoxycinnamate approximately 4-methoxycinnamate approximately 3-hydroxycinnamate > hydrocaffeate approximately 4-hydroxycinnamate > ferulate > 2-hydroxycinnamate > caffeate approximately sinapate. With respect to the position of the hydroxy substituents at the phenyl moiety, the transesterification activity of C. antarctica lipase B increased in the order meta > para > ortho. The immobilized lipases from Rhizomucor miehei and Thermomyces lanuginosus demonstrated moderate and low transesterification activity, respectively. Compounds with inverse chemical structure, that is, 3-phenylpropyl alkanoates such as 3-(4-hydroxyphenyl)propyl oleate and 3-(3,4-dimethoxyphenyl)propyl oleate, were obtained by C. antarctica lipase-catalyzed transesterification of fatty acid methyl esters with the corresponding 3-phenylpropan-1-ols in high yield, as well.

  9. Solvent-free one-pot cyclization and acetylation of chalcones: Synthesis of some 1-acetyl pyrazoles and spectral correlations of 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones

    Directory of Open Access Journals (Sweden)

    G. Thirunarayanan

    2016-11-01

    Full Text Available One-pot synthesis of some 1N-acetyl pyrazoles including 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones has been achieved via solvent-free microwave irradiation using substituted chalcones, hydrazine hydrate and acetic anhydride in the presence of catalytic amount of fly-ash: PTS catalyst. The yield of these 1N-acetyl pyrazole derivatives is more than 75%. The synthesized 1N-acetyl pyrazoline derivatives were characterized by their physical constants and spectral data. The infrared spectral νCN and CO (cm−1 frequencies, NMR chemical shifts (δ, ppm of Ha, Hb, Hc, CH3 protons, CN, CO and CH3 carbons of 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones have been assigned and correlated with Hammett substituent constants and Swain-Lupton’s parameters using single and multi-regression analysis. From the results of statistical analyses, the effect of substituents on the above group frequencies and chemical shifts of the acetylated pyrazoles were discussed.

  10. Kinetic study of lipase-catalyzed glycerolysis of palm olein using Lipozyme TLIM in solvent-free system.

    Directory of Open Access Journals (Sweden)

    Thomas Shean Yaw Choong

    Full Text Available Diacylglycerol (DAG and monoacylglycerol (MAG are two natural occurring minor components found in most edible fats and oils. These compounds have gained increasing market demand owing to their unique physicochemical properties. Enzymatic glycerolysis in solvent-free system might be a promising approach in producing DAG and MAG-enriched oil. Understanding on glycerolysis mechanism is therefore of great importance for process simulation and optimization. In this study, a commercial immobilized lipase (Lipozyme TL IM was used to catalyze the glycerolysis reaction. The kinetics of enzymatic glycerolysis reaction between triacylglycerol (TAG and glycerol (G were modeled using rate equation with unsteady-state assumption. Ternary complex, ping-pong bi-bi and complex ping-pong bi-bi models were proposed and compared in this study. The reaction rate constants were determined using non-linear regression and sum of square errors (SSE were minimized. Present work revealed satisfactory agreement between experimental data and the result generated by complex ping-pong bi-bi model as compared to other models. The proposed kinetic model would facilitate understanding on enzymatic glycerolysis for DAG and MAG production and design optimization of a pilot-scale reactor.

  11. Fly-ash:H2SO4 catalyzed solvent free efficient synthesis of some aryl chalcones under microwave irradiation

    Science.gov (United States)

    Thirunarayanan, G.; Mayavel, P.; Thirumurthy, K.

    2012-06-01

    Some 2E aryl chalcones have been synthesized using greener catalyst Fly-ash:H2SO4 assisted solvent free environmentally benign Crossed-Aldol reaction. The yields of chalcones are more than 90%. The synthesized chalcones are characterized by their physical constants and spectral data.

  12. [Au]/[Pd] Multicatalytic Processes: Direct One-Pot Access to Benzo[ c ]chromenes and Benzo[ b ]furans

    KAUST Repository

    Oonishi, Yoshihiro

    2014-08-28

    A new synthetic protocol that combines the advantages offered by eco-friendly solvent-free reactions and sequential transformations is reported. This strategy offers straightforward access to benzo[c]chromenes and benzo[b]furans from commercially available starting materials. This two-step, one-pot strategy consists of an Au-catalyzed hydrophenoxylation process followed by Pd-catalyzed C-H activation or Mizoroki-Heck reactions. The selectivity of the process towards C-H activation or Mizoroki-Heck reaction can be easily tuned. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Poly(4-VinylpyridiniumHydrogen Sulfate Catalyzed an Efficient and Ecofriendly Protocol for the One-Pot Multicomponent Synthesis of 1,8-Acridinediones in Aqueous Medium

    Directory of Open Access Journals (Sweden)

    Janardhan Banothu

    2013-01-01

    Full Text Available Highly efficient, ecofriendly, and improved protocol for the synthesis of 1,8-acridinediones has been developed via one-pot multicomponent condensation of 1,3-cyclohexanedione/dimedone, aromatic aldehydes, and ammonium acetate utilizing poly(4-vinylpyridiniumhydrogen sulfate as catalyst in aqueous medium. Excellent yields in shorter reaction time, simple work-up procedure, easy recovery, and reusability of the catalyst are attractive features of this green protocol.

  14. Solvent-Free Lipase-Catalyzed Synthesis of Technical-Grade Sugar Esters and Evaluation of Their Physicochemical and Bioactive Properties

    Directory of Open Access Journals (Sweden)

    Ran Ye

    2016-05-01

    Full Text Available Technical-grade oleic acid esters of sucrose and fructose were prepared using solvent-free biocatalysis at 65 °C, without any downstream purification applied, and their physicochemical and bioactivity-related properties were evaluated and compared to a commercially available sucrose laurate emulsifier. To increase the conversion of sucrose and fructose oleate, prepared previously using solvent-free lipase-catalyzed esterification catalyzed by Rhizomucor miehei lipase (81% and 83% ester, respectively, the enzymatic reaction conditions was continued using CaSO4 to control the reactor’s air headspace and a lipase (from Candida antarctica B with a hydrophobic immobilization matrix to provide an ultralow water activity, and high-pressure homogenation, to form metastable suspensions of 2.0–3.3 micron sized saccharide particles in liquid-phase reaction media. These measures led to increased ester content of 89% and 96% for reactions involving sucrose and fructose, respectively. The monoester content among the esters decreased from 90% to <70% due to differences in regioselectivity between the lipases. The resultant technical-grade sucrose and fructose lowered the surface tension to <30 mN/m, and possessed excellent emulsification capability and stability over 36 h using hexadecane and dodecane as oils, comparable to that of sucrose laurate and Tween® 80. The technical-grade sugar esters, particularly fructose oleate, more effectively inhibited gram-positive foodborne pathogens (Lactobacillus plantarum, Pediococcus pentosaceus and Bacillus subtilis. Furthermore, all three sugar esters displayed antitumor activity, particularly the two sucrose esters. This study demonstrates the importance of controlling the biocatalysts’ water activity to achieve high conversion, the impact of a lipase’s regioselectivity in dictating product distribution, and the use of solvent-free biocatalysis to important biobased surfactants useful in foods, cosmetics

  15. YCl3-Catalyzed Highly Selective Ring Opening of Epoxides by Amines at Room Temperature and under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Wuttichai Natongchai

    2017-11-01

    Full Text Available A simple, efficient, and environmentally benign approach for the synthesis of β-amino alcohols is herein described. YCl3 efficiently carried out the ring opening of epoxides by amines to produce β-amino alcohols under solvent-free conditions at room temperature. This catalytic approach is very effective, with several aromatic and aliphatic oxiranes and amines. A mere 1 mol % concentration of YCl3 is enough to deliver β-amino alcohols in good to excellent yields with high regioselectivity.

  16. Enantioselective Solvent-Free Synthesis of 3-Alkyl-3-hydroxy-2-oxoindoles Catalyzed by Binam-Prolinamides

    Directory of Open Access Journals (Sweden)

    Abraham Bañn-Caballero

    2015-07-01

    Full Text Available BINAM-prolinamides are very efficient catalyst for the synthesis of non-protected and N-benzyl isatin derivatives by using an aldol reaction between ketones and isatins under solvent-free conditions. The results in terms of diastereo- and enantioselectivities are good, up to 99% de and 97% ee, and higher to those previously reported in the literature under similar reaction conditions. A high variation of the results is observed depending on the structure of the isatin and the ketone used in the process. While 90% of ee and 97% ee, respectively, is obtained by using (Ra-BINAM-l-(bisprolinamide as catalyst in the addition of cyclohexanone and α-methoxyacetone to free isatin, 90% ee is achieved for the reaction between N-benzyl isatin and acetone using N-tosyl BINAM-l-prolinamide as catalyst. This reaction is also carried out using a silica BINAM-l-prolinamide supported catalyst under solvent-free conditions, which can be reused up to five times giving similar results.

  17. Solvent-Free Biginelli Reactions Catalyzed by Hierarchical Zeolite Utilizing a Ball Mill Technique: A Green Sustainable Process

    Directory of Open Access Journals (Sweden)

    Ameen Shahid

    2017-03-01

    Full Text Available A sustainable, green one-pot process for the synthesis of dihydropyrimidinones (DHPMs derivatives by a three-component reaction of β-ketoester derivatives, aldehyde and urea or thiourea over the alkali-treated H-ZSM-5 zeolite under ball-milling was developed. Isolation of the product with ethyl acetate shadowed by vanishing of solvent was applied. The hierachical zeolite catalyst (MFI27_6 showed high yield (86%–96% of DHPMs in a very short time (10–30 min. The recyclability of the catalyst for the subsequent reactions was examined in four subsequent runs. The catalyst was shown to be robust without a detectable reduction in catalytic activity, and high yields of products showed the efficient protocol of the Biginelli reactions.

  18. Brønsted acidic ionic liquid catalyzed an efficient and eco-friendly protocol for the synthesis of 2,4,5-trisubstituted-1H-imidazoles under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Janardhan Banothu

    2017-05-01

    Full Text Available A simple, highly efficient and eco-friendly protocol for the synthesis of 2,4,5-trisubstituted-1H-imidazoles via one-pot three component condensation of benzil/benzoin, aldehydes and ammonium acetate under solvent-free conditions has been achieved utilizing Brønsted acidic ionic liquid, (4-sulfobutyltris(4-sulfophenyl phosphonium hydrogen sulfate as catalyst. The remarkable features of this methodology are excellent yields in shorter reaction times, cleaner reaction profile, and environmentally benign nature, use of non-toxic, readily synthesizable, inexpensive and recyclable catalyst.

  19. Functionalized SBA-15 supported nickel (II)–oxime–imine catalysts for liquid phase oxidation of olefins under solvent-free conditions

    International Nuclear Information System (INIS)

    Paul, Luna; Banerjee, Biplab; Bhaumik, Asim; Ali, Mahammad

    2016-01-01

    A new oxime–imine functionalized highly ordered mesoporous SBA-15 (SBA-15-NH 2 -DAMO) has been synthesized via post-synthesis functionalization of SBA-15 with 3-aminopropyl-triethoxysilane followed by the Schiff base condensation with diacetylmonooxime, which was further reacted with Ni(ClO 4 ) 2 to yield the functionalized nickel catalyst SBA-15-NH 2 -DAMO-Ni. All the synthesized materials were thoroughly characterized using different characterization techniques. It was found that SBA-15-NH 2 -DAMO-Ni catalyzes the one-pot oxidation of olefins like styrene, cyclohexene, cyclooctene, 1-hexene and 1-octene to the corresponding benzaldehyde, cyclohexene-1-ol and cyclooctene-oxide, respectively under solvent-free conditions by using tert-butylhydroperoxide as oxidant. - Graphical abstract: A new well characterized oxime–imine functionalized highly ordered mesoporous SBA-15-NH 2 -DAMO-Ni complex catalyzes the one-pot oxidation of olefins under solvent free mild conditions.

  20. One-pot synthesis of 2H-pyrans by indium(III) chloride-catalyzed reactions. efficient synthesis of pyranocoumarins, pyranophenalenones, and pyranoquinolinones

    International Nuclear Information System (INIS)

    Lee, Yong Rok; Kim, Do Hoon; Shim, Jae Jin; Kim, Seog K.; Park, Jung Hag; Cha, Jin Soon; Lee, Chong Soon

    2002-01-01

    An efficient synthesis of 2H-pyrans is achieved by indium (III) chloride-catalyzed reactions of 1,3-dicarbonyl compounds with a variety of α.β-unsaturated aldehydes in moderates yields. This method has been applied to the synthesis of pyranocoumarins, pyranophenaleneones, and pyranoquinolinone alkaloids

  1. N-Heterocyclic Carbene Catalyzed [3+2] Cycloaddition of Enals with Masked Cinnamates for the Asymmetric One-Pot Synthesis of Adipic Acid Derivatives.

    Science.gov (United States)

    Chen, Xiang-Yu; Li, Sun; Sheng, He; Liu, Qiang; Jafari, Ehsan; von Essen, Carolina; Rissanen, Kari; Enders, Dieter

    2017-09-21

    A novel short entry to 3,4-disubstituted adipic acids has been developed by employing an asymmetric NHC-catalyzed [3+2] cycloaddition of enals with masked cinnammates in moderate to good yields and high stereoselectivities. The synthetic utility of the protocol was demonstrated by the basic conversion of the masked cyclopentanone intermediates to 3S,4S-disubstituted adipic acid precursors of pharmaceutically important gababutins. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. One-Pot Synthesis of Some New Pyrido[2,3-d]pyrimidine Derivatives Catalyzed by Sodium Lauryl Sulfate in Aqueous Media

    Directory of Open Access Journals (Sweden)

    Sheng-Hui Li

    2010-01-01

    Full Text Available A series of pyrido[2,3-d]pyrimidine derivatives were synthesized by the three-component reaction of aromatic aldehyde, malononitrile and 6-amino-4-hydroxy-2-mercaptopyrimidine catalyzed by sodium lauryl sulfate (SDS in aqueous media. It was interesting that further aromatization took place automatically. This method provides several advantages such as easier work-up, milder reaction conditions and environmental friendly.

  3. Dual response surface-optimized process for feruloylated diacylglycerols by selective lipase-catalyzed transesterification in solvent free system.

    Science.gov (United States)

    Zheng, Yan; Wu, Xiao-Mei; Branford-White, Christopher; Quan, Jing; Zhu, Li-Min

    2009-06-01

    Feruloylated diacylglycerol (FDAG) was synthesized using a selective lipase-catalyzed the transesterification between ethyl ferulate and triolein. To optimize the reaction conversion and purity of FDAG, dual response surface was applied to determine the effects of five-level-five-factors and their reciprocal interactions on product synthesis. A total of 32 individual experiments were performed to study reaction temperature, reaction time, substrate molar ratio, enzyme loading, and water activity. The highest reaction conversion and selectivity towards FDAG were 73.9% and 92.3%, respectively, at 55 degrees C, reaction time 5.3 day, enzyme loading 30.4 mg/ml, water activity 0.08, and a substrate molar ratio of 3.7. Moreover, predicted values showed good validation with the experimental values when experiments corresponding to selected points on the contour plots were carried out.

  4. Perlite-SO3H nanoparticles as an efficient and reusable catalyst for one-pot three-component synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives under both microwave-assisted and thermal solvent-free conditions: Single crystal X-ray structure analysis and theoretical study

    Directory of Open Access Journals (Sweden)

    Ali Ramazani

    2016-01-01

    Full Text Available A general synthetic route for the synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives has been developed using perlite-SO3H nanoparticles as efficient catalyst under both microwave-assisted and thermal solvent-free conditions. The combination of 2-naphthol, aldehyde and urea enabled the synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives in the presence of perlite-SO3H nanoparticles in good to excellent yields. This method provides several advantages like simple work-up, environmentally benign, and shorter reaction times along with high yields. In order to explore the recyclability of the catalyst, the perlite-SO3H nanoparticles in solvent-free conditions were used as catalyst for the same reaction repeatedly and the change in their catalytic activity was studied. It was found that perlite-SO3H nanoparticles could be reused for four cycles with negligible loss of their activity. Single crystal X-ray structure analysis and theoretical studies also were investigated for 4i product. The electronic properties of the compound have been analyzed using DFT calculations (B3LYP/6-311+G*. The FMO analysis suggests that charge transfer takes place within the molecule and the HOMO is localized mainly on naphthalene and oxazinone rings whereas the LUMO resides on the naphthalene ring.

  5. Preparation of lipophilic alkyl (hydroxy)benzoates by solvent-free lipase-catalyzed esterification and transesterification.

    Science.gov (United States)

    Vosmann, K; Wiege, B; Weitkamp, P; Weber, N

    2008-08-01

    Long-chain alkyl benzoates, e.g., lauryl 4-hydroxybenzoate, palmityl 4-hydroxybenzoate, and oleyl 4-hydroxy-3-methoxybenzoate, are formed in high to moderate conversion by lipase-catalyzed transesterification of the corresponding short-chain alkyl benzoates (0.3 to 1 mmol) with fatty alcohols in an equimolar ratio. The substrates are reacted in vacuo in the absence of solvents and drying agents in the reaction mixture. Immobilized lipase B from Candida antarctica (Novozym 435) demonstrates higher activity for the transesterification of various methyl (hydroxy)benzoates with long-chain alcohols than for the corresponding esterification reactions. For example, transesterification activity is around 25-fold higher than esterification activity for the preparation of oleyl 4-hydroxybenzoate. The relative transesterification activities of methoxy- and hydroxy-substituted methyl benzoates found for Novozym 435 are as follows: 2-methoxybenzoate approximately 3-methoxybenzoate > 4-methoxybenzoate > 3-hydroxybenzoate approximately 2-hydroxybenzoate > 4-hydroxybenzoate approximately 4-hydroxy-3-methoxybenzoate approximately 3-hydroxy-4-methoxybenzoate > > 3,4-dihydroxybenzoate. With respect to the position of the substituents at the phenyl moiety of methyl benzoates, transesterification activity of Novozym 435 increases in the order ortho approximately meta > para. Compounds with inverse chemical structure, e.g., (methoxy)benzyl alkanoates, are formed in much higher rates both by esterification and transesterification than the analogous alkyl benzoates. Purification by deacidification, crystallization, or vacuum distillation yielded 74% to 89% of the reaction products.

  6. Ultrasound-promoted one-pot three component synthesis of tetrazoles catalyzed by zinc sulfide nanoparticles as a recyclable heterogeneous catalyst.

    Science.gov (United States)

    Naeimi, Hossein; Kiani, Fatemeh

    2015-11-01

    Ultrasound irradiation was applied for the appropriate and rapid synthesis of 1-substituted tetrazoles through cyclization reaction of various primary amines, sodium azide and triethyl orthoformate. This reaction was effectively catalyzed by ZnS nanoparticles as an efficient, recoverable and reusable catalyst. Compared with conventional methods, this method has the considerable advantages such as shorter reaction times, easier work-up, purer products with high yields and mild conditions. The ZnS nanoparticles catalyst is an excellent instance to replace Brønsted acids for the preparation of 1-substituted tetrazole derivatives in very short reaction times with excellent yields. The catalyst can be recovered and reused several times without significant loss of its catalytic activity. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Solvent-free lipase-catalyzed preparation of diglycerides from co-products of vegetable oil refining

    Directory of Open Access Journals (Sweden)

    Tangkam, Kamol

    2008-09-01

    Full Text Available Co-products of vegetable oil refining such as a mixed deodorizer distillate resulting from the refining of various vegetable oils, a crude distillate resulting from the physical refining of coconut oil and commercial mixtures of distilled sunflower and coconut fatty acids were used as starting materials for the enzymatic preparation of diglycerides. Reaction conditions (temperature, pressure, molar ratio for the formation of diglycerides by lipase-catalyzed esterification/transesterification were studied using the mixed deodorizer distillate and glycerol as starting materials. The best results were obtained with the immobilized lipase B from Candida antarctica (Novozym 435 in vacuo at 60 °C leading to moderate proportions (~52% of diglycerides. The proportion of diglycerides increased when residual acylglycerides of the co-products of vegetable oil refining were hydrolyzed prior to esterification. Thus, the esterification of hydrolyzed co-products of vegetable oil refining with glycerol led to high formation (62-72% of diglycerides. Short-path vacuum distillation of the esterification products yielded distillation residues containing from 70% to 94% diglycerides. The proportions of fatty acids and monoglycerides in the distilled residues were quite low (Subproductos del refinado de los aceites vegetales tales como el destilado obtenido en el desodorizador al refinar distintos aceites vegetales, el destilado crudo resultante de la refinación física del aceite de coco, y mezclas comerciales de los ácidos grasos obtenidos en la destilación de aceites de girasol y coco fueron utilizados como materiales de partida para la preparación enzimática de diglicéridos. Se estudiaron las condiciones de reacción (temperatura, presión, relación molar para la formación de diglicéridos mediante esterificación/ transesterificación catalizada por lipasas usando la mezcla obtenida del desodorizador y glicerol como materiales de partida. Los mejores

  8. An Efficient Synthesis of 3,4-Dihydropyrimidin-2(1H-Ones and Thiones Catalyzed by a Novel Brønsted Acidic Ionic Liquid under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Yonghong Zhang

    2015-02-01

    Full Text Available We report here an efficient and green method for Biginelli condensation reaction of aldehydes, β-ketoesters and urea or thiourea catalyzed by Brønsted acidic ionic liquid [Btto][p-TSA] under solvent-free conditions. Compared to the classical Biginelli reaction conditions, the present method has the advantages of giving good yields, short reaction times, near room temperature conditions and the avoidance of the use of organic solvents and metal catalyst.

  9. Benign and efficient preparation of thioethers by solvent-free S-alkylation of thiols with alkyl halides catalyzed by potassium fluoride on alumina

    DEFF Research Database (Denmark)

    Nguyen, Kha Ngoc; Duus, Fritz; Luu, Thi Xuan Thi

    2016-01-01

    The preparation of thioethers by S-alkylation of various thiols with alkyl halides under solvent-free reaction conditions using potassium fluoride on alumina (KF/Al2O3) as a solid catalyst has been investigated in detail with respect to three different modes of reaction activation (ultrasound...

  10. Microwave-Enhanced Sulphated Zirconia and SZ/MCM-41 Catalyzed Regioselective Synthesis of β-Amino Alcohols Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Eduardo González-Zamora

    2008-04-01

    Full Text Available A solvent-free approach for the regioselective synthesis of β-amino alcohols inshorter reaction times and higher yields, compared to conventional heating is described. Itinvolves microwave (MW exposure of undiluted reactants in the presence of sulphatedzirconia (SZ or sulphated zirconia over MCM-41 (SZM as catalyst. Both acid materialscan be easily recovered and reused.

  11. One-pot Reductive Amination of Carbonyl Compounds with NaBH4 ...

    Indian Academy of Sciences (India)

    Abstract. An efficient one-pot procedure for the direct reductive amination of aldehyde and ketones was achieved in the presence of sodium borohydride by using B(OSO3H)3/SiO2(SBSA) as the reusable solid cat- alyst in acetonitrile and solvent-free conditions. Both aromatic and aliphatic aldehyde reacted well to give the.

  12. One-pot Reductive Amination of Carbonyl Compounds with NaBH₄ ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 129; Issue 1. One-pot Reductive Amination of Carbonyl Compounds with NaBH₄-B(OSO₃H)₃/SiO₂ in Acetonitrile and in Solvent-free Condition. HOSEIN HAMADI SAMIRA JAVADI. Regular Article Volume 129 Issue 1 January 2017 pp 75-80 ...

  13. One-pot efficient green synthesis of 1,4-dihydro-quinoxaline-2,3

    Indian Academy of Sciences (India)

    3-dione (1) has been achieved in a one-pot reaction at room temperature from substituted -phenylene diamine and oxalic acid under solvent-free conditions by a simple grinding method with unsurpassed atom economy. Thermal and powder ...

  14. Microwave assisted highly efficient one-pot multi-component synthesis of novel 2-(tetrasubstituted-1H-pyrrol-3-yl-4H-chroman-4-ones catalyzed by heterogeneous reusable silica gel supported polyphosphoric acid (PPA/SiO2

    Directory of Open Access Journals (Sweden)

    Sumit Kumar

    2018-02-01

    Full Text Available A solvent-free, eco-friendly and facile approach for the synthesis of highly functionalized tetrasubstituted pyrroles has been reported through one-pot four-component reaction of aldehyde, amine, nitroalkane and 1,3-diketone using silica gel supported polyphosphoric acid (PPA–SiO2 under microwave condition. The reaction occured through the in situ formation of β-keto enamine and nitrostyrene analog following Michael addition and finally intramolecular annulation affording the products in good yields. The key features of the present method include clean reaction, mild conditions, low catalyst loading, straightforward, high to excellent yields, short reaction time, avoiding use of harmful metal catalyst and organic solvent, environmentally friendly compared to the existing methods, recovery and reusability of catalyst and easy workup procedure.

  15. Solvent-free one-pot 1,3-dipolar cycloaddition reactions of ...

    Indian Academy of Sciences (India)

    esting part is 1,3-dipolar cycloaddition, which repre- sents one of the most versatile tools for the construction of five-membered heterocycles. Owing to the labile na- ... (300 MHz, FT NMR) using TMS as internal standard. 13C NMR spectra were recorded on the same instrument at 75MHz. The coupling constants (J) are given ...

  16. Solvent-free one-pot 1,3-dipolar cycloaddition reactions of ...

    Indian Academy of Sciences (India)

    Int. Ed. 43 6250. 3. Perreux L and Loupy A 2001 Tetrahedron 57 9199. 4. Loupy A, Petti A, Hamelin J, Texier-Boullet F, Jacquault. P and Mathé D 1998 Synthesis 9 1213. 5. Loupy A 2006 Microwaves in organic synthesis. (Weinheim, Germany: Wiley-VCH) 2nd edn. 6. Kabalka G W and Pagni R M 1997 Tetrahedron 53 7999.

  17. Facile solvent-free one-pot synthesis of pyranobenzopyrans and ...

    Indian Academy of Sciences (India)

    Organic Chemistry Research Laboratory, Ramnarain Ruia College, Matunga, Mumbai 400 019, India e-mail: pednekarsuhas@gmail.com. MS received 9 December 2010; revised 8 May ... terial, antifungal, CNS depressant, antiviral, ulcer inhibitor, etc.16–22 Suksdorfin and DCK which contain pyranobenzopyran moiety are ...

  18. Synthesis of Azanucleosides through Regioselective Ring-Opening of Epoxides Catalyzed by Sulphated Zirconia under Microwave and Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Guillermo E. Negrón-Silva

    2012-03-01

    Full Text Available New azanucleosides were obtained using sulphated zirconia (ZS as catalyst in the nucleophilic oxirane ring opening reaction of 1-allyl-3-(oxiran-2-ylmethyl pyrimidine-2,4(1H,3H-dione and 1-allyl-5-methyl-3-(oxiran-2-ylmethyl-pyrimidine-2,4(1H,3H-dione, with (S-prolinol. The new templates were obtained with good yields following a route which exploits the reactivity of epoxides in the presence of sulphated zirconia as catalyst. The key step was carried out using microwave and solvent-free conditions and proceeds with high selectivity.

  19. One-Pot Three-Step Synthesis of 1,2,3-Triazoles by Copper-Catalyzed Cycloaddition of Azides with Alkynes formed by a Sonogashira Cross-Coupling and Desilylation

    Science.gov (United States)

    Friscourt, Frédéric; Boons, Geert-Jan

    2010-01-01

    A microwave-assisted one-pot, three-step Sonogashira cross coupling-desilylation-cycloaddition sequence was developed for the convenient preparation of 1,4-disubstituted 1,2,3-triazoles starting from a range of halides, acyl chlorides, ethynyltrimethylsilane and azides. PMID:20942390

  20. Solvent-Free Biodiesel Production Catalyzed by Crude Lipase Powder from Seeds: Effects of Alcohol Polarity, Glycerol, and Thermodynamic Water Activity.

    Science.gov (United States)

    Kouteu, Paul Alain Nanssou; Blin, Joël; Baréa, Bruno; Barouh, Nathalie; Villeneuve, Pierre

    2017-10-04

    The aim of this work was to evaluate the potential of crude lipase powders made from Adansonia grandidieri and Jatropha mahafalensis seeds for the synthesis of fatty acid alkyl esters in a solvent-free system. The influence of the nature of the alcohol, the amount of glycerol, and hydration of the powder was investigated. Results showed that the activity of these crude lipase powders was inversely proportional to the alcohol polarity and the amount of the glycerol in the reaction medium. To ensure optimum activity, A. grandidieri and J. mahafalensis powders must be conditioned to a water activity of 0.33 and 0.66. To obtain a fatty acid ethyl ester yield greater than 95% with A. grandidieri, ethanol should be introduced at an amount corresponding to a triacylglycerol to ethanol molar ratio of 2:1 every 15 h for 96 h and use 25% of preconditioned crude lipase powders (2 additions of 12.5%).

  1. short communication one-pot synthesis of 2,4,5-trisubstituted

    African Journals Online (AJOL)

    L-Proline: An efficient catalyst for the one-pot synthesis of 2,4,5-trisubstituted and 1,2,4,5- tetrasubstituted imidazoles. Tetrahedron 2009, 65, 10155-10161. 9. (a) Balalaei, S.; Arabanian, A. One-pot synthesis of tetrasubstituted imidazoles catalyzed by zeolite HY and silica gel under microwave irradiation. Green Chem. 2000 ...

  2. One-pot conversion of biomass to chemicals

    OpenAIRE

    Baumgarten, Björn Frederik

    2017-01-01

    One-pot conversion of biomass to diols can be a simple and fast alternative to other methods of biomass conversion. The catalyst for this conversion is required to be bifunctional, catalysing both hydrogenation and retro-aldol condensations. Hydrogenation is realized by usage of transition metals like Ru, Ni and alternativly copper. Retro-aldol condensations are catalyzed by various tungsten compounds, amphoteric and basic metal oxides or basic sites. New amphoteric and basic catalysts ...

  3. Facile one-pot four component synthesis of pyrido[2,3-d:6,5-d‧]dipyrimidines catalyzed by CuFe2O4 magnetic nanoparticles in water

    Science.gov (United States)

    Naeimi, Hossein; Didar, Asieh

    2017-06-01

    A simple, efficient and green method for the synthesis of pyrido[2,3-d:6,5-d‧]dipyrimidine derivatives via one-pot four-component reaction of aromatic aldehyde, 2-thiobarbituric acid, ammonium acetate in the presence of catalytic amount of a magnetically heterogeneous catalyst has been developed. This protocol includes some important advantages such as; high to excellent product yields, high atom economy, usage of water as a green reaction medium, reusability of catalyst, and simple work-up procedure.

  4. One-pot Sequential Reactions Featuring a Copper-catalyzed Amination Leading to Pyrido[2',1':2,3]imidazo[4,5-c]quinolines and Dihydropyrido[2',1':2,3]imidazo[4,5-c]quinolines.

    Science.gov (United States)

    Fan, Xue-Sen; Zhang, Ju; Li, Bin; Zhang, Xin-Ying

    2015-06-01

    Tetracyclic skeletons combining an imidazo[1,2-a]pyridine moiety with a quinoline framework such as pyrido[2',1':2,3]imidazo[4,5-b]quinoline are stimulating increasing interests since they are close isosteres of a series of powerful antiproliferative compounds. In this paper, we report a novel methodology for the synthesis of pyrido[2',1':2,3]imidazo[4,5-c]quinolines through one-pot sequential reactions of commercially available or readily obtainable 2-aminopyridines, 2-bromophenacyl bromides, aqueous ammonia, and aldehydes. Moreover, dihydropyrido[2',1':2,3]imidazo[4,5-c]quinolines could also be obtained in a similar manner by using various ketones as the substrates in place of aldehydes. Notably, the whole procedure combines condensation/amination/cyclization reactions in one pot to give complex compounds in a simple and practical manner. Compared with literature methods, the synthetic strategy reported herein has the advantages of readily available starting materials, structural diversity of products, good functional group tolerance, and obviation of step-by-step operations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Parameters affecting incorporation and by-product formation during the production of structured phospholipids by lipase-catalyzed acidolysis in solvent free system

    DEFF Research Database (Denmark)

    Vikbjerg, Anders Falk; Mu, Huiling; Xu, Xuebing

    2005-01-01

    By-product formation is a serious problem in the lipase-catalyzed acyl exchange of phospholipids (PL). By-products are formed due to parallel hydrolysis reactions and acyl migration in the reaction system. A clear elucidation of these side reactions is important for practical operation in order t...

  6. One-Pot Eco-Safe Saccharin-Catalyzed Procedure for Expedient and Convenient Synthesis of Dihydropyrano[2,3-c]pyrazole, Tetrahydrobenzo[b]pyran and Pyrano[2,3-d]pyrimidinone Scaffolds as a Green and Versatile Catalyst

    Directory of Open Access Journals (Sweden)

    Farzaneh Mohamadpour

    2018-02-01

    Full Text Available A green and facile saccharin-catalyzed procedure is developed for the one-pot convenient synthesis of dihydropyrano[2,3-c]pyrazole, tetrahydrobenzo[b]pyran and pyrano[2,3-d]pyrimidinone scaffolds via multi-component tandem Knoevenagel cyclocondensation reaction. This procedure has the chief advantages of green, inexpensive and readily available catalyst, high atom-economy, high to quantitative yields and the reaction procedure is mild and involves facile workup procedure to obtain the desired products in short reaction times.

  7. Functionalized SBA-15 supported nickel (II)–oxime–imine catalysts for liquid phase oxidation of olefins under solvent-free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Luna [Department of Chemistry, Jadavpur University, Kolkata 700 032 (India); Banerjee, Biplab [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Bhaumik, Asim, E-mail: msab@iacs.res.in [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Ali, Mahammad, E-mail: m_ali2062@yahoo.com [Department of Chemistry, Jadavpur University, Kolkata 700 032 (India)

    2016-05-15

    A new oxime–imine functionalized highly ordered mesoporous SBA-15 (SBA-15-NH{sub 2}-DAMO) has been synthesized via post-synthesis functionalization of SBA-15 with 3-aminopropyl-triethoxysilane followed by the Schiff base condensation with diacetylmonooxime, which was further reacted with Ni(ClO{sub 4}){sub 2} to yield the functionalized nickel catalyst SBA-15-NH{sub 2}-DAMO-Ni. All the synthesized materials were thoroughly characterized using different characterization techniques. It was found that SBA-15-NH{sub 2}-DAMO-Ni catalyzes the one-pot oxidation of olefins like styrene, cyclohexene, cyclooctene, 1-hexene and 1-octene to the corresponding benzaldehyde, cyclohexene-1-ol and cyclooctene-oxide, respectively under solvent-free conditions by using tert-butylhydroperoxide as oxidant. - Graphical abstract: A new well characterized oxime–imine functionalized highly ordered mesoporous SBA-15-NH{sub 2}-DAMO-Ni complex catalyzes the one-pot oxidation of olefins under solvent free mild conditions.

  8. PEG1000-Based Dicationic Acidic Ionic Liquid Catalyzed One-Pot Synthesis of 4-Aryl-3-Methyl-1-Phenyl-1H-Benzo[h]pyrazolo [3,4-b]quinoline-5,10-Diones via Multicomponent Reactions

    Directory of Open Access Journals (Sweden)

    Yi-Ming Ren

    2015-09-01

    Full Text Available A novel and green approach for efficient and rapid synthesis of 4-aryl-3-methyl-1-phenyl-1H-benzo[h]pyrazolo[3,4-b]quinoline-5,10-diones has been accomplished by the one-pot condensation reaction of aromatic aldehydes, 3-methyl-1-phenyl-1H-pyrazol-5-amine and 2-hydroxynaphthalene-1,4-dione using PEG1000-based dicationic acidic ionic liquid (PEG1000-DAIL as a catalyst was reported. Recycling studies have shown that the PEG1000-DAIL can be readily recovered and reused several times without significant loss of activity. The key advantages are the short reaction time, high yields, simple workup, and recovered catalyst.

  9. Solvent-free copper-catalyzed click chemistry for the synthesis of N-heterocyclic hybrids based on quinoline and 1,2,3-triazole

    Directory of Open Access Journals (Sweden)

    Martina Tireli

    2017-11-01

    Full Text Available Copper-catalyzed mechanochemical click reactions using Cu(II, Cu(I and Cu(0 catalysts have been successfully implemented to provide novel 6-phenyl-2-(trifluoromethylquinolines with a phenyl-1,2,3-triazole moiety at O-4 of the quinoline core. Milling procedures proved to be significantly more efficient than the corresponding solution reactions, with up to a 15-fold gain in yield. Efficiency of both solution and milling procedures depended on the p-substituent in the azide reactant, resulting in H < Cl < Br < I reactivity bias. Solid-state catalysis using Cu(II and Cu(I catalysts entailed the direct involvement of the copper species in the reaction and generation of highly luminescent compounds which hindered in situ monitoring by Raman spectroscopy. However, in situ monitoring of the milling processes was enabled by using Cu(0 catalysts in the form of brass milling media which offered a direct insight into the reaction pathway of mechanochemical CuAAC reactions, indicating that the catalysis is most likely conducted on the surface of milling balls. Electron spin resonance spectroscopy was used to determine the oxidation and spin states of the respective copper catalysts in bulk products obtained by milling procedures.

  10. Laccase-catalyzed C-S and C-C coupling for a one-pot synthesis of 1,4-naphthoquinone sulfides and 1,4-naphthoquinone sulfide dimers

    CSIR Research Space (South Africa)

    Wellington, Kevin W

    2013-06-01

    Full Text Available Oxidative C-S and C-C bond formation with aryl and alkyl thiols was catalyzed under mild conditions in a reaction vessel open to air at pH 4.5 in the presence of a commercial laccase (Novozym 51003 or Suberase) and a cosolvent (DMF) to afford 1,4...

  11. Rh(I)-catalyzed transformation of propargyl vinyl ethers into (E,Z)-dienals: stereoelectronic role of trans effect in a metal-mediated pericyclic process and a shift from homogeneous to heterogeneous catalysis during a one-pot reaction.

    Science.gov (United States)

    Vidhani, Dinesh V; Krafft, Marie E; Alabugin, Igor V

    2014-01-03

    The combination of experiments and computations reveals unusual features of stereoselective Rh(I)-catalyzed transformation of propargyl vinyl ethers into (E,Z)-dienals. The first step, the conversion of propargyl vinyl ethers into allene aldehydes, proceeds under homogeneous conditions via a "cyclization-mediated" mechanism initiated by Rh(I) coordination at the alkyne. This path agrees well with the small experimental effects of substituents on the carbinol carbon. The key feature revealed by the computational study is the stereoelectronic effect of the ligand arrangement at the catalytic center. The rearrangement barriers significantly decrease due to the greater transfer of electron density from the catalytic metal center to the CO ligand oriented trans to the alkyne. This effect increases electrophilicity of the metal and lowers the calculated barriers by 9.0 kcal/mol. Subsequent evolution of the catalyst leads to the in situ formation of Rh(I) nanoclusters that catalyze stereoselective tautomerization. The intermediacy of heterogeneous catalysis by nanoclusters was confirmed by mercury poisoning, temperature-dependent sigmoidal kinetic curves, and dynamic light scattering. The combination of experiments and computations suggests that the initially formed allene-aldehyde product assists in the transformation of a homogeneous catalyst (or "a cocktail of catalysts") into nanoclusters, which in turn catalyze and control the stereochemistry of subsequent transformations.

  12. A One-Pot Oxidation/Enantioselective Oxa-Michael Cascade

    NARCIS (Netherlands)

    Willemsen, Jorgen S.; Megens, Rik P.; Roelfes, Gerard; van Hest, Jan C. M.; Rutjes, Floris P. J. T.

    A laccase/(2,2,6,6-tetramethylpiperidin-1-yl)oxy (TEMPO) mediated oxidation was combined with an aqueous, enantioselective copper-catalyzed Michael addition reaction of water in one pot. The copper catalyst was also immobilized onto DNA to induce enantioselectivity in the reaction. Low conversions

  13. KSF-SUPPORTED HETEROPOLY ACIDS CATALYZED ONE-POT ...

    African Journals Online (AJOL)

    Preferred Customer

    this transformation [7-24], have been used to circumvent some of the problems associated with the classical ... coupled plasma (ICP) atomic emission spectroscopy on a Spectro Ciros CCd spectrometer. (Germany). The morphology of supported catalyst was studied by scanning electron microscopy. (SEM) using XL30 ...

  14. NANO CRYSTALLINE ZnO CATALYZED ONE POT THREE ...

    African Journals Online (AJOL)

    Also some of them have displayed a remarkable assay in the treatment of important diseases including .... can be a vital role for the formation of the desired product. So, the optimization of amount of the .... Soc. Ethiop. 2016, 30(2). 295. The role of nano-ZnO catalyst in reaction was the activation of carbonyl groups. This.

  15. Three Component Synthesis of Substituted 4H-[1,3]Dioxin Derivatives Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Hosseini-Tabatabaei

    2012-01-01

    Full Text Available Reaction between aryl aldehydes, acetylacetone and alkyl isocyanides in solvent-free conditions provided a simple and efficient one-pot route for the synthesis of 1-(2-alkylamino-6-methyl-4-aryl-4H-[1,3]dioxin-5-ylethanone derivatives in excellent yields.

  16. A Green One-Pot Synthesis of 4-Hydroxychromenylarylmethyl- 6-Hydroxypyrimidine-2,4-Diones Using Titanium Dioxide Nanowires as an Effective and Recyclable Catalyst.

    Science.gov (United States)

    Eskandari, Khalil; Karami, Bahador

    2016-01-01

    Since a wide range of biological and pharmaceutical activities of barbituric acid, 4-hydroxycoumarin and their derivatives have been disclosed until now, in the domain of our interest to find newly catalytic routes for highly efficient synthesis of potentially interesting biologically active organic compounds, and extension of their areas, herein we introduce a three component combinatorial reaction based on (N,N-dimethyl)barbituric acid and 4- hydroxycoumarin scaffolds. All starting materials were purchased from Merck chemical company and were applied without further purifications. Catalytic reaction between barbituric acid (or N,N-dimethyl barbituric acid), 4-hydroxycoumarin, and a wide range of aryl aldehydes by employing titanium dioxide nanowires (TiO2 NWs) is successfully performed under solvent-free conditions at 100 °C, and led efficiently to obtain target products. From loading above mentioned three component reaction, starting materials in the presence of catalytic amounts of TiO2 NWs as a key factor were condensed together via three C-C bond formation to obtain 12 newly prepared compounds. This procedure profits some advantages such as an efficiency, environmental safety and high recyclability of nano-catalyst. In this work, by the use of a green adapted method in a condensation three component reaction catalyzed by TiO2 NWs as an efficient nano-catalyst, some newly prepared products were prepared in a one pot, and the scope of potentially interesting biologically active organic compounds which can be duly considered by biologists and pharmacologists was developed.

  17. Sulfonated polynaphthalene as an effective and reusable catalyst for the one-pot preparation of amidoalkyl naphthols: DFT and spectroscopic studies

    Science.gov (United States)

    Pourmousavi, Seied Ali; Moghimi, Parvin; Ghorbani, Fatemeh; Zamani, Mehdi

    2017-09-01

    Sulfonated polynaphthalene (S-PNP) as a carbon-based solid acid efficiently catalyzed the one-pot three-component synthesis of amidoalkyl naphthols. The three-component process of substituted aryl aldehydes, 2-naphthol, and amide (benzamide and acetamide) or urea in the presence of S-PNP under thermal solvent-free conditions is described. Short reaction times, high yields and easy work-up are the advantages of this protocol. Furthermore, the catalyst can be readily recycled and reused without obvious significant loss of activity. Also, density functional theory (DFT) with the aid of M06-2X and B3LYP methods was used for studying of the optimized structure, molecular orbitals, electrostatic potential (ESP) map and spectroscopic analysis of some selected amidoalkyl naphthols. The thermochemical parameters of reactions including enthalpy, internal energy, entropy and Gibbs free energy were also investigated. The theoretically calculated infrared (IR) and 1H nuclear magnetic resonance (NMR) spectra of title compounds were compared to the experimental data. Based on the results, the synthesis of amidoalkyl naphthols is exothermic. A good consistency between the calculated and observed spectral data was found.

  18. Zeolite H-BEA catalysed multicomponent reaction: One-pot ...

    Indian Academy of Sciences (India)

    BEA catalysed multicomponent reaction: One-pot synthesis of amidoalkyl naphthols - Biologically active drug-like molecules. Sunil R Mistry Rikesh S Joshi Kalpana C Maheria. Volume 123 Issue 4 July 2011 pp 427-432 ...

  19. Application of sulfonic acid functionalized nanoporous silica (SBA-Pr-SO3H in the green one-pot synthesis of triazoloquinazolinones and benzimidazoquinazolinones

    Directory of Open Access Journals (Sweden)

    Ghodsi Mohammadi Ziarani

    2015-01-01

    Full Text Available Sulfonic acid functionalized SBA-15 (SBA-Pr-SO3H with a pore size of 6 nm was proven to be an efficient heterogeneous nanoporous solid acid catalyst in the green one-pot synthesis of triazoloquinazolinones and benzimidazoquinazolinones from the reaction of aromatic aldehydes with 3-amino-1,2,4-triazole (or 2-aminobenzimidazole and dimedone under solvent free conditions.

  20. A Facile Solvent Free Microwave Induced Synthesis and Antibacterial Activity of Some 3-(2’-Hydroxyphenyl-5-(Substituted Aryl-2-Pyrazoline-N1-Caboxaldehydes

    Directory of Open Access Journals (Sweden)

    Birbal Bajia

    2007-01-01

    Full Text Available A novel one pot formylation of 3-(2’-hydroxyphenyl-5-(substituted 2-pyrazolines has been carried out using microwave irradiation with formic acid. solvent free reaction afforded title compounds in 80-90% yield with high purity.synthesized compounds were tested for their antibacterial activity using standard drug.

  1. One pot glucose detection by [Fe(III)(biuret-amide)] immobilized on mesoporous silica nanoparticles: an efficient HRP mimic.

    Science.gov (United States)

    Malvi, Bharmana; Panda, Chakadola; Dhar, Basab B; Gupta, Sayam Sen

    2012-05-28

    An [Fe(III)(biuret-amide)] complex has been immobilized onto mesoporous silica nanoparticles via Cu(I) catalyzed azide-alkyne click chemistry. This hybrid material functions as an efficient peroxidase mimic and was successfully used for the quantitative determination of hydrogen peroxide and glucose via a one-pot colorimetric assay. This journal is © The Royal Society of Chemistry 2012

  2. Silica Gel-Mediated Organic Reactions under Organic Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Satoaki Onitsuka

    2012-09-01

    Full Text Available Silica gel was found to be an excellent medium for some useful organic transformations under organic solvent-free conditions, such as (1 the Friedel-Crafts-type nitration of arenes using commercial aqueous 69% nitric acid alone at room temperature, (2 one-pot Wittig-type olefination of aldehydes with activated organic halides in the presence of tributyl- or triphenylphosphine and Hunig’s base, and (3 the Morita-Baylis-Hillman reaction of aldehydes with methyl acrylate. After the reactions, the desired products were easily obtained in good to excellent yields through simple manipulation.

  3. Zeolite H-BEA catalysed multicomponent reaction: One-pot ...

    Indian Academy of Sciences (India)

    lent thermal stability which make them economically and environmentally feasible.2 The use of zeolites as a ... of zeolite H-BEA was added. The mixture was stirred under thermal solvent-free condition at 120. ◦. C in oil bath for 5–7min and the reaction was followed by. TLC. After completion of reaction, mass was cooled to.

  4. Solvent-free fluidic organic dye lasers.

    Science.gov (United States)

    Choi, Eun Young; Mager, Loic; Cham, Tran Thi; Dorkenoo, Kokou D; Fort, Alain; Wu, Jeong Weon; Barsella, Alberto; Ribierre, Jean-Charles

    2013-05-06

    We report on the demonstration of liquid organic dye lasers based on 9-(2-ethylhexyl)carbazole (EHCz), so-called liquid carbazole, doped with green- and red-emitting laser dyes. Both waveguide and Fabry-Perot type microcavity fluidic organic dye lasers were prepared by capillary action under solvent-free conditions. Cascade Förster-type energy transfer processes from liquid carbazole to laser dyes were employed to achieve color-variable amplified spontaneous emission and lasing. Overall, this study provides the first step towards the development of solvent-free fluidic organic semiconducting lasers and demonstrates a new kind of optoelectronic applications for liquid organic semiconductors.

  5. An environmentally benign one pot synthesis of substituted ...

    Indian Academy of Sciences (India)

    Instance of Plagiarism in Journal of Chemical Sci- ences and withdrawal of published article. The Journal of Chemical Sciences office received a complaint from an alert reader to the effect that the paper 'An environmentally benign one pot syn- thesis of substituted quinolines catalysed by fluo- roboric acid based ionic ...

  6. Supporting information A practical one-pot synthesis of azides ...

    Indian Academy of Sciences (India)

    user

    1. Supporting information. A practical one-pot synthesis of azides directly from alcohols. Lalthazuala Rokhum and Ghanashyam Bez*. Department of Chemistry, North Eastern Hill University, Shillong-793022, India bez@nehu.ac.in ; ghanashyambez@yahoo.com. Page 2-16. 1HNMR & 13CNMR spectra of new compounds ...

  7. One-pot synthesis of quinaldine derivatives by using microwave ...

    Indian Academy of Sciences (India)

    Abstract. A convenient and efficient procedure for synthesis of quinaldine derivatives has been developed by a simple one-pot reaction of aniline derivatives and acetaldehyde on the surface of neutral alumina impregnated with hydrochloric acid under microwave irradiation without any solvent according to green chemistry.

  8. Microwave assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Dr.P.T.P

    Microwave assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents. C PRAVEEN a. , A NANDAKUMAR a. , P DHEENKUMAR b. , D MURALIDHARAN a and P T. PERUMAL a,. * a. Organic Chemistry Division, Central Leather Research Institute, Adyar, Chennai 600020,. Tamilnadu, India.

  9. Microwave-assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Microwave-assisted synthesis of benzothiazole and benzoxazole libraries via PIFA promoted cyclocondensation of 2-aminothiophenols/2-aminophenols with aldehydes under one-pot condition in good to excellent yields was achieved. Twenty compounds have been investigated for their analgesic activity and showed ...

  10. Nickel nanoparticles: A highly efficient catalyst for one pot synthesis ...

    Indian Academy of Sciences (India)

    J. Chem. Sci. Vol. 124, No. 4, July 2012, pp. 907–912. c Indian Academy of Sciences. Nickel nanoparticles: A highly efficient catalyst for one pot synthesis of tetraketones and biscoumarins ... Department of Chemistry, University of Delhi, Delhi 110 007, India e-mail: ... and for the synthesis of various heterocyclic com-.

  11. Microwave-assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 124; Issue 3 ... Abstract. Microwave-assisted synthesis of benzothiazole and benzoxazole libraries via PIFA promoted cyclocondensation of 2-aminothiophenols/2-aminophenols with aldehydes under one-pot condition in good to excellent yields was achieved. Twenty ...

  12. Two expedient 'one-pot'methods for synthesis of -aryl- ...

    Indian Academy of Sciences (India)

    Keywords. -aryl--mercaptoketones; anhydrous potassium carbonate; amberlyst-15; chalcones; thia-Michael addition. Abstract. Two expedient one-pot methods have been developed for synthesis of -aryl--mercaptoketones using acetophenones, benzaldehydes and thiols as starting materials. The methods involve ...

  13. An environmentally benign one pot synthesis of substituted ...

    Indian Academy of Sciences (India)

    Organic synthesis generally required large amount of solvent, avoiding the use of organic solvents in synthesis is a paradigm shift directed at developing more benign chemistry, and with ionic liquids surprisingly can lead to access to new compounds. An elegant one-pot synthesis of quinoline derivatives has been achieved ...

  14. Microwave assisted one-pot synthesis of benzothiazole and ...

    Indian Academy of Sciences (India)

    Dr.P.T.P

    1. Microwave assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents. C PRAVEEN a. , A NANDAKUMAR a. , P DHEENKUMAR b. , D MURALIDHARAN a and P T. PERUMAL a,. * a. Organic Chemistry Division, Central Leather Research Institute, Adyar, Chennai 600020,. Tamilnadu ...

  15. SHORT COMMUNICATION A NOVEL ONE-POT SYNTHESIS OF ...

    African Journals Online (AJOL)

    Preferred Customer

    Nano zinc oxide was explored as a heterogeneous and reusable catalyst for the one-pot synthesis of spirooxindoles via three-component reaction between urea, isatin, and 1,3-dicarbonyl compounds. KEY WORDS: Nano-ZnO, Spirooxindoles, Isatin. INTRODUCTION. The indole skeleton occurs in many important natural ...

  16. One-pot multi-component green synthesis of highly substituted piperidines

    Directory of Open Access Journals (Sweden)

    Ravi Bansal

    2017-05-01

    Full Text Available An effective and expeditious method of the synthesis of a highly functionalized piperidines, catalyzed by nontoxic, recyclable and environment friendly sodium lauryl sulfate (SLS, via one-pot multi-component condensation of aldehydes, amines and β-ketoesters in water at room temperature, has been developed. This new protocol has advantages such as moderate to high yields of products obtained after simple post reaction workup. Structure of the synthesized compounds 4a–4j have been elucidated based on the 1H NMR, 13C NMR, FT-IR spectroscopy and elemental analysis.

  17. Layered materials with coexisting acidic and basic sites for catalytic one-pot reaction sequences.

    Science.gov (United States)

    Motokura, Ken; Tada, Mizuki; Iwasawa, Yasuhiro

    2009-06-17

    Acidic montmorillonite-immobilized primary amines (H-mont-NH(2)) were found to be excellent acid-base bifunctional catalysts for one-pot reaction sequences, which are the first materials with coexisting acid and base sites active for acid-base tamdem reactions. For example, tandem deacetalization-Knoevenagel condensation proceeded successfully with the H-mont-NH(2), affording the corresponding condensation product in a quantitative yield. The acidity of the H-mont-NH(2) was strongly influenced by the preparation solvent, and the base-catalyzed reactions were enhanced by interlayer acid sites.

  18. Enantioselective solvent-free Robinson annulation reactions

    Indian Academy of Sciences (India)

    Unknown

    The use of proline or any other amino acid in asymmetric annulation reactions in a solid–liquid phase reaction in the absence of solvents to effect an asymmetric synthesis is an important step forward towards cleaner synthesis 2. ... Reports on solvent-free reactions have become increasingly frequent and the field has.

  19. An Environmentally Friendly Solvent-free Synthesis of 3,4 ...

    African Journals Online (AJOL)

    NICO

    An Environmentally Friendly Solvent-free Synthesis of. 3,4-Dihydropyrimidinones using a p-Aminobenzene. Sulfonic Acid Catalyzed Biginelli Reaction. Ming Shu Wu,a,b,* Ping Heb and Xiang Zhu Zhanga. aDepartment of Chemical Engineering, Institute of Anyang Technology, Anyang, 455000, Henan, P.R. China.

  20. Multicomponent, Solvent-Free Synthesis of 1-Amidoalkyl-2-naphthols in the Presence of H3+xPMo12-x Vx O40 Heteropolyacids as Recyclable and Green Catalysts

    Directory of Open Access Journals (Sweden)

    Fatemeh F. Bamoharram

    2011-01-01

    Full Text Available A rapid and efficient one-pot method for the synthesis of 1-amidoalkyl-2-naphthols has been developed in the presence of mixed-addenda vanadium(V-substituted polyoxomolybdates including: H3+xPMo12-xVxO40 (x=1-3 heteropolyacids (HPAs as recyclable catalysts under solvent-free conditions. In all cases heteropolyacid with x = 3 gave the highest yield under solvent-free conditions.

  1. Optically active thiophenes via an organocatalytic one-pot methodology.

    Science.gov (United States)

    Ransborg, Lars Krogager; Albrecht, Łukasz; Weise, Christian F; Bak, Jesper R; Jørgensen, Karl Anker

    2012-02-03

    A general methodology for the synthesis of trisubstituted, optically active thiophenes by an organocatalytic one-pot reaction cascade is presented. The target products are synthesized in good yields (up to 92%) and with excellent enantioselectivities (up to 98% ee). Importantly, based on practical and easily available starting materials, the presented methodology can be conducted under mild reaction conditions. To further elucidate the generality, the synthesis of optically active thienoindoles, as well as selenophenes, is also demonstrated. © 2012 American Chemical Society

  2. Dynamics of solvent-free grafted nanoparticles

    KAUST Repository

    Chremos, Alexandros

    2012-01-01

    The diffusivity and structural relaxation characteristics of oligomer-grafted nanoparticles have been investigated with simulations of a previously proposed coarse-grained model at atmospheric pressure. Solvent-free, polymer-grafted nanoparticles as well as grafted nanoparticles in a melt were compared to a reference system of bare (ungrafted) particles in a melt. Whereas longer chains lead to a larger hydrodynamic radius and lower relative diffusivity for grafted particles in a melt, bulk solvent-free nanoparticles with longer chains have higher relative diffusivities than their short chain counterparts. Solvent-free nanoparticles with short chains undergo a glass transition as indicated by a vanishing diffusivity, diverging structural relaxation time and the formation of body-centered-cubic-like order. Nanoparticles with longer chains exhibit a more gradual increase in the structural relaxation time with decreasing temperature and concomitantly increasing particle volume fraction. The diffusivity of the long chain nanoparticles exhibits a minimum at an intermediate temperature and volume fraction where the polymer brushes of neighboring particles overlap, but must stretch to fill the interparticle space. © 2012 American Institute of Physics.

  3. Sequential decarboxylative azide–alkyne cycloaddition and dehydrogenative coupling reactions: one-pot synthesis of polycyclic fused triazoles

    Directory of Open Access Journals (Sweden)

    Kuppusamy Bharathimohan

    2014-12-01

    Full Text Available Herein, we describe a one-pot protocol for the synthesis of a novel series of polycyclic triazole derivatives. Transition metal-catalyzed decarboxylative CuAAC and dehydrogenative cross coupling reactions are combined in a single flask and achieved good yields of the respective triazoles (up to 97% yield. This methodology is more convenient to produce the complex polycyclic molecules in a simple way.

  4. One pot synthesis of 2-hydroxy pyrrolidine derivatives

    Directory of Open Access Journals (Sweden)

    Putta. P. Varma

    2011-01-01

    Full Text Available One pot reaction of various 2-amino-thiadiazoles or thiazoles and 2,3- dihydrofuran under mild condition in presence of CeCl 3.7H 2O as catalyst transformed the amino group of 2-amino-thiadiazoles or thiazoles into a medicinally important 2-hydroxy pyrrolidine ring system in good to excellent yields. The generality of the reaction was sufficiently investigated and demonstrated. The new reaction path way for this conversion was established by spectroscopic and analytical methods.

  5. Facile synthesis of 1-naphthol azo dyes with nano SiO2/HIO4 under solvent-free conditions

    OpenAIRE

    A.R. Pourali; A. Bamoniri; S.M.R. Nazifi

    2013-01-01

    Nano-silica supported periodic acid (nano-SPIA) has been utilized as a heterogeneous reagent for a highly efficient and one pot synthesis of azo dyes based on 1-naphthol under solvent-free conditions at room temperature. This method has some advantages, the reaction workup is very easy and the catalyst can be easily separated from the reaction mixture and one-pot procedure. The related products have been obtained in good to excellent yields, high purity and short reaction times. The structure...

  6. One-pot reaction for the preparation of biofunctionalized self-assembled monolayers on gold surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Raigoza, Annette F.; Fies, Whitney; Lim, Amber; Onyirioha, Kristeen; Webb, Lauren J., E-mail: lwebb@cm.utexas.edu

    2017-02-01

    Highlights: • One-pot synthesis of α-helical-terminated self-assembled monolayers on Au(111). • Synthesis of high density, structured, and covalently bound α-helices on Au(111). • Characterization by surface-averaged and single molecule techniques. • Peptide-terminated surfaces for fabrication of biomaterials and sensors. - Abstract: The Huisgen cycloaddition reaction (“click” chemistry) has been used extensively to functionalize surfaces with macromolecules in a straightforward manner. We have previously developed a procedure using the copper(I)-catalyzed click reaction to tether synthetic α-helical peptides carrying two alkyne groups to a well-ordered azide-terminated alkanethiol self-assembled monolayer (SAM) on a Au(111) surface. While convenient, click-based strategies potentially pose significant problems from reagents, solvents, and reaction temperatures that may irreversibly damage some molecules or substrates. Tuning click chemistry conditions would allow individual optimization of reaction conditions for a wide variety of biomolecules and substrate materials. Here, we explore the utility of simultaneous SAM formation and peptide-attachment chemistry in a one-pot reaction. We demonstrate that a formerly multistep reaction can be successfully carried out concurrently by mixing azide-terminated alkanethiols, CuCl, and a propargylglycine-containing peptide over a bare gold surface in ethanol and reacting at 70 °C. X-ray photoelectron spectroscopy (XPS), surface infrared spectroscopy, surface circular dichroic (CD) spectroscopy, and scanning tunneling microscopy (STM) were used to determine that this one-pot reaction strategy resulted in a high density of surface-bound α-helices without aggregation. This work demonstrates the simplicity and versatility of a SAM-plus-click chemistry strategy for functionalizing Au surfaces with structured biomolecules.

  7. One-pot multienzyme (OPME) systems for chemoenzymatic synthesis of carbohydrates

    Science.gov (United States)

    Yu, Hai; Chen, Xi

    2016-01-01

    Glycosyltransferase-catalyzed enzymatic and chemoenzymatic syntheses are powerful approaches for the production of oligosaccharides, polysaccharides, glycoconjugates, and their derivatives. Enzymes involved in the biosynthesis of sugar nucleotide donors can be combined with the glycosyltransferases in one pot for efficient production of target glycans from simple monosaccharides and accpetors. The identification of enzymes involved in the salvage pathway of sugar nucleotide generation has greatly facilitate the development of simplified and efficient one-pot multienzyme (OPME) systems for synthesizing major glycan epitopes in mammalian glycomes. The applications of OPME methods are steadily gaining popularity mainly due to the increasing availability of wild-type and engineered enzymes. Substrate promiscuity of these enzymes and their mutants allows OPME synthesis of carbohydrates with naturally occurring post-glycosylational modificiation (PGMs) and their non-natural derivatives using modified monosaccharides as precursors. The OPME systems can be applied in sequential for synthesizing complex carbohydrates. The sequence of the sequential OPME processes, the glycosyltransferase used, and the substrate specificities of glycosyltransferasese define the structures of the products. The OPME and sequential OPME strategies can be extended to diverse glycans in other glycomes when suitable enzymes with substrate promiscuity become available. The Perspective summariezes the work of the authors and collaborators on the development of glycosyltransferase-based OPME systems for carbohydrate synthesis. Future directions are also discussed. PMID:26881499

  8. One-pot multienzyme (OPME) systems for chemoenzymatic synthesis of carbohydrates.

    Science.gov (United States)

    Yu, Hai; Chen, Xi

    2016-03-14

    Glycosyltransferase-catalyzed enzymatic and chemoenzymatic syntheses are powerful approaches for the production of oligosaccharides, polysaccharides, glycoconjugates, and their derivatives. Enzymes involved in the biosynthesis of sugar nucleotide donors can be combined with glycosyltransferases in one pot for efficient production of the target glycans from simple monosaccharides and acceptors. The identification of enzymes involved in the salvage pathway of sugar nucleotide generation has greatly facilitated the development of simplified and efficient one-pot multienzyme (OPME) systems for synthesizing major glycan epitopes in mammalian glycomes. The applications of OPME methods are steadily gaining popularity mainly due to the increasing availability of wild-type and engineered enzymes. Substrate promiscuity of these enzymes and their mutants allows OPME synthesis of carbohydrates with naturally occurring post-glycosylational modifications (PGMs) and their non-natural derivatives using modified monosaccharides as precursors. The OPME systems can be applied in sequence for synthesizing complex carbohydrates. The sequence of the sequential OPME processes, the glycosyltransferase used, and the substrate specificities of the glycosyltransferases define the structures of the products. The OPME and sequential OPME strategies can be extended to diverse glycans in other glycomes when suitable enzymes with substrate promiscuity become available. This Perspective summarizes the work of the authors and collaborators on the development of glycosyltransferase-based OPME systems for carbohydrate synthesis. Future directions are also discussed.

  9. Solvent-free and room temperature synthesis of 3-arylquinolines from different anilines and styrene oxide in the presence of Al2O3/MeSO3H

    Directory of Open Access Journals (Sweden)

    Hashem Sharghi

    2017-09-01

    Full Text Available A highly efficient, simple and environmentally friendly synthesis of 3-arylquinolines has been developed in the presence of Al2O3/MeSO3H via one-pot reaction of anilines and styrene oxide. This methodology provides very rapid access to 3-arylquinolines in good to excellent yields under solvent-free conditions at room temperature in air.

  10. A New One-Pot Synthesis of Quinoline-2-carboxylates under Heterogeneous Conditions.

    Science.gov (United States)

    Gabrielli, Serena; Giardinieri, Alessandra; Sampaolesi, Susanna; Ballini, Roberto; Palmieri, Alessandro

    2016-06-15

    Quinoline-2-carboxylates are an important subclass of quinoline derivatives largely present in a variety of biologically active molecules, as well as useful ligands in metal-catalyzed reactions. Herein, we present a new one-pot protocol for synthesizing this class of derivatives starting from β-nitroacrylates and 2-aminobenzaldehydes. In order to optimize the protocol, we investigated several reaction conditions, obtaining the best results using the 2-tert-Butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine (BEMP) as solid base, in acetonitrile. Finally, we demonstrated the generality of our approach over several substrates which led to synthesize a plethora of functionalized quinolines-2-carboxylate derivatives in good overall yields.

  11. Environmentally friendly efficient one-pot esterification of cyclohexane with CuO-promoted sulfated zirconia.

    Science.gov (United States)

    Wang, Jingjing; Ma, Hongzhu; Wang, Bo

    2008-09-15

    The production of dibutyl phthalate directly from oxidation and esterification of cyclohexane, catalyzed by CuO-modified sulfated zirconia (SZCu) by one-pot under mild condition, was studied. The esterification reaction process was monitored by UV-vis spectra and the distribution of the products was analyzed by gas chromatograph-mass spectrometry (GC-MS). The result revealed that the SZCu catalyst was efficient in the direct oxidation and esterification of cyclohexane to ester. The selectivity for ester (dibutyl phthalate) can reach up to 72.2 wt.%, and the yield of ester was 29.5 wt.%. The esterification reaction, that offers several advantages such as usage of environmental friendly oxidant, simple work-up procedure, no-solvent conditions, short reaction times, easy recovery and reusability of the catalyst, is necessary for chemosynthesis industry from the environment standpoint. The regeneration property of SZCu was also tested in this work.

  12. Solvent free lipase catalyzed synthesis of butyl caprylate

    Indian Academy of Sciences (India)

    To achieve maximum conversion theoptimum parameters thus established include; temperature 60 ◦C, mole ratio of caprylic acid and butanol as 1:2, lipase loading 2% (w/v), 250 rpm speed of agitation and 4g of molecular sieves. The immobilized enzyme wasalso recycled and reused for 7 cycles with only 30% loss from its ...

  13. Solvent free lipase catalyzed synthesis of butyl caprylate

    Indian Academy of Sciences (India)

    MEERA T SOSE

    2017-11-10

    Nov 10, 2017 ... C, mole ratio of caprylic acid and butanol as 1:2, lipase loading 2% (w/v), 250 rpm speed of agitation and 4g of molecular sieves. The immobilized enzyme was also recycled and reused for 7 cycles with only 30% loss from its initial activity. The thermodynamic parameters at different temperatures were also ...

  14. Facile synthesis of 1-naphthol azo dyes with nano SiO2/HIO4 under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    A.R. Pourali

    2013-09-01

    Full Text Available Nano-silica supported periodic acid (nano-SPIA has been utilized as a heterogeneous reagent for a highly efficient and one pot synthesis of azo dyes based on 1-naphthol under solvent-free conditions at room temperature. This method has some advantages, the reaction workup is very easy and the catalyst can be easily separated from the reaction mixture and one-pot procedure. The related products have been obtained in good to excellent yields, high purity and short reaction times. The structures of the products have been characterized by several techniques using UV-Vis, FT-IR, 1H NMR, 13C NMR and mass spectra.DOI: http://dx.doi.org/10.4314/bcse.v27i3.13

  15. An Efficient Solvent-Free Protocol for the Synthesis of 1-Amidoalkyl-2-naphthols using Silica-Supported Molybdatophosphoric Acid

    Directory of Open Access Journals (Sweden)

    Abdolkarim Zare

    2010-01-01

    Full Text Available A highly efficient, green and simple solvent-free method for the synthesis of 1-amidoalkyl-2-naphthols via one-pot multi-components condensation of 2-naphthol, aromatic aldehydes and amides in the presence of catalytic amount of silica-supported molybdatophosphoric acid (H3PMo12O40.xH2O/SiO2, 3.17 mol% is described. The reactions proceed rapidly and the title compounds are produced in high to excellent yields.

  16. Oligoquinolines under Solvent-free Microwave Irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Park, Kwi-Jeon; Kwon, Tae-Woo [Kyungsung University, Busan (Korea, Republic of)

    2015-01-15

    Quinolines are thermally stable and can be used as an excellent n-type semiconducting materials. Since quinolines are also known to be electron acceptor molecules, combination of various electron donor building blocks can be utilized in photonic and electronic organic light-emitting diode (OLED) applications. For example, donor.acceptor systems with phenothiazine (or carbazole) molecules as electron donors and the phenylquinoline group as an electron acceptor provide an efficient approach for the design of new materials exhibiting highly efficient charge-transfer photophysics and electroluminescence in OLEDs. We have described the Friedlander quinoline synthesis between aminobenzophenones and symmetrical diacetyl compounds having phenothiazine, carbazole, biphenyl, and phenyl moieties under solvent-free microwave irradiation in 12.98% isolated yields.

  17. An efficient one-pot four-segment condensation method for protein chemical synthesis.

    Science.gov (United States)

    Tang, Shan; Si, Yan-Yan; Wang, Zhi-Peng; Mei, Kun-Rong; Chen, Xin; Cheng, Jing-Yuan; Zheng, Ji-Shen; Liu, Lei

    2015-05-04

    Successive peptide ligation using a one-pot method can improve the efficiency of protein chemical synthesis. Although one-pot three-segment ligation has enjoyed widespread application, a robust method for one-pot four-segment ligation had to date remained undeveloped. Herein we report a new one-pot multisegment peptide ligation method that can be used to condense up to four segments with operational simplicity and high efficiency. Its practicality is demonstrated by the one-pot four-segment synthesis of a plant protein, crambin, and a human chemokine, hCCL21. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Mild one-pot Horner-Wadsworth-Emmons olefination and intramolecular N-arylation for the syntheses of indoles, all regio-isomeric azaindoles, and thienopyrroles.

    Science.gov (United States)

    Choi, Ji Hye; Lim, Hwan Jung

    2015-05-14

    The syntheses of various N-protected aromatic-ring fused pyrrole-2-carboxylate derivatives have been accomplished using mild one-pot Horner-Wadsworth-Emmons olefination and Cu-catalyzed intramolecular N-arylation reactions. The optimized mild one-pot reaction conditions of various 2-bromo arylcarboxaldehydes with commercially available N-protected phosphonoglycine trimethylesters gave the desired aromatic-ring fused pyrrole-2-carboxylates, such as substituted indole-, all regio-isomeric azaindole-, and thienopyrrole-2-carboxylates, in good to excellent yields. These conditions showed broad substrate compatibility, without the loss of the protecting group.

  19. 147 ONE POT METHOD FOR THE SYNTHESIS OF ARYLIDENE ...

    African Journals Online (AJOL)

    The reactivity of condensing aldehyde is an important factor in the synthesis. Presence of alcohol enhances the formation of products. This fact have been utilized for alkali catalyzed synthesis of many arylidene flavanones been reported by them. The special feature of long conjugation with 4-keto group of flavanone moiety.

  20. Solvent-Free Production of Bioflavors by Enzymatic Esterification of Citronella (Cymbopogon winterianus) Essential Oil.

    Science.gov (United States)

    Paroul, Natália; Grzegozeski, Luana Paula; Chiaradia, Viviane; Treichel, Helen; Cansian, Rogério L; Oliveira, J Vladimir; de Oliveira, Débora

    2012-01-01

    Enzymatic esterification of citronella essential oil towards the production of geranyl and citronellyl esters may present great scientific and technological interest due to the well-known drawbacks of the chemical-catalyzed route. In this context, this work reports the maximization of geranyl and citronellyl esters production by esterification of oleic and propionic acids in a solvent-free system using a commercial immobilized lipase as catalyst. Results of the reactions showed that the strategy adopted for the experimental design proved to be useful in evaluating the effects of the studied variables on the reaction conversion using Novozym 435 as catalyst. The operating conditions that maximized the production of each ester were determined, leading, in a general way, to conversions of about 90% for all systems. New experimental data on enzymatic esterification of crude citronella essential oil for geranyl and citronellyl esters production in solvent-free system are reported in this work.

  1. One-Pot Synthesis of (+-Nootkatone via Dark Singlet Oxygenation of Valencene: The Triple Role of the Amphiphilic Molybdate Catalyst

    Directory of Open Access Journals (Sweden)

    Bing Hong

    2016-11-01

    Full Text Available Efficient one-pot catalytic synthesis of (+-nootkatone was performed from (+-valencene using only hydrogen peroxide and amphiphilic molybdate ions. The process required no solvent and proceeded in three cascade reactions: (i singlet oxygenation of valencene according to the ene reaction; (ii Schenck rearrangement of one hydroperoxide into the secondary β-hydroperoxide; and (iii dehydration of the hydroperoxide into the desired (+-nootkatone. The solvent effect on the hydroperoxide rearrangement is herein discussed. The amphiphilic dimethyldioctyl ammonium molybdate, which is also a balanced surfactant, played a triple role in this process, as molybdate ions catalyzed at both Step 1 and Step 3 and it allowed the rapid formation of a three-phase microemulsion system that highly facilitates product recovery. Preparative synthesis of the high added value (+-nootkatone was thus performed at room temperature with an isolated yield of 46.5%. This is also the first example of a conversion of allylic hydroperoxides into ketones catalyzed by molybdate ions.

  2. Organic Synthesis under Solvent-free Condition. An Environmentally ...

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 7; Issue 11. Organic Synthesis under Solvent-free Condition: An Environmentally Benign Procedure – II. Gopalpur Nagendrappa. General Article Volume 7 Issue 11 November 2002 pp 64-69 ...

  3. One-pot glycosylations in the synthesis of human milk oligosaccharides

    DEFF Research Database (Denmark)

    Jennum, Camilla Arboe; Fenger, Thomas Hauch; Bruun, Linda Maria

    2014-01-01

    Human milk oligosaccharides contain a well-defined core structure that makes them interesting synthetic targets for one-pot glycosylation strategies. In this investigation, a one-pot procedure was studied in which a galactose thioglycoside is coupled chemoselectively to a phthalimide...

  4. One-pot conversion of cellulose to ethylene glycol with multifunctional tungsten-based catalysts.

    Science.gov (United States)

    Wang, Aiqin; Zhang, Tao

    2013-07-16

    With diminishing fossil resources and increasing concerns about environmental issues, searching for alternative fuels has gained interest in recent years. Cellulose, as the most abundant nonfood biomass on earth, is a promising renewable feedstock for production of fuels and chemicals. In principle, the ample hydroxyl groups in the structure of cellulose make it an ideal feedstock for the production of industrially important polyols such as ethylene glycol (EG), according to the atom economy rule. However, effectively depolymerizing cellulose under mild conditions presents a challenge, due to the intra- and intermolecular hydrogen bonding network. In addition, control of product selectivity is complicated by the thermal instabilities of cellulose-derived sugars. A one-pot catalytic process that combines hydrolysis of cellulose and hydrogenation/hydrogenolysis of cellulose-derived sugars proves to be an efficient way toward the selective production of polyols from cellulose. In this Account, we describe our efforts toward the one-pot catalytic conversion of cellulose to EG, a typical petroleum-dependent bulk chemical widely applied in the polyester industry whose annual consumption reaches about 20 million metric tons. This reaction opens a novel route for the sustainable production of bulk chemicals from biomass and will greatly decrease the dependence on petroleum resources and the associated CO₂ emission. It has attracted much attention from both industrial and academic societies since we first described the reaction in 2008. The mechanism involves a cascade reaction. First, acid catalyzes the hydrolysis of cellulose to water-soluble oligosaccharides and glucose (R1). Then, oligosaccharides and glucose undergo C-C bond cleavage to form glycolaldehyde with catalysis of tungsten species (R2). Finally, hydrogenation of glycolaldehyde by a transition metal catalyst produces the end product EG (R3). Due to the instabilities of glycolaldehyde and cellulose

  5. β–Cyclodextrin–Propyl Sulfonic Acid Catalysed One-Pot Synthesis of 1,2,4,5-Tetrasubstituted Imidazoles as Local Anesthetic Agents

    Directory of Open Access Journals (Sweden)

    Yan Ran

    2015-11-01

    Full Text Available Some functionalized 1,2,4,5-tetrasubstituted imidazole derivatives were synthesized using a one-pot, four component reaction involving 1,2-diketones, aryl aldehydes, ammonium acetate and substituted aromatic amines. The synthesis has been efficiently carried out in a solvent free medium using β-cyclodextrin-propyl sulfonic acid as a catalyst to afford the target compounds in excellent yields. The local anesthetic effect of these derivatives was assessed in comparison to lidocaine as a standard using a rabbit corneal and mouse tail anesthesia model. The three most potent promising compounds were subjected to a rat sciatic nerve block assay where they showed considerable local anesthetic activity, along with minimal toxicity. Among the tested analogues, 4-(1-benzyl-4,5-diphenyl-1H-imidazol-2-yl-N,N-dimethylaniline (5g was identified as most potent analogue with minimal toxicity. It was further characterized by a more favourable therapeutic index than the standard.

  6. Facile One-Pot Synthesis of Amidoalkyl Naphthols and Benzopyrans Using Magnetic Nanoparticle-Supported Acidic Ionic Liquid as a Highly Efficient and Reusable Catalyst

    Directory of Open Access Journals (Sweden)

    Qiang Zhang

    2017-11-01

    Full Text Available An efficient and eco-friendly procedure for the synthesis of 1-amidoalkyl-2-naphthol and tetrahydrobenzo[b]pyran derivatives has been developed through a one-pot three-component condensation of aldehydes with 2-naphthol and amides, or with malononitrile and dimedone in the presence of magnetic nanoparticle supported acidic ionic liquid (AIL@MNP as a novel heterogeneous catalyst under solvent-free conditions. This new procedure offers several advantages such as short reaction time, excellent yields, operational simplicity and without any tedious work-up for catalyst recovery or product purification. Moreover, the catalyst could be simply separated by an external magnet and reused six times without significant loss of catalytic activity.

  7. Organocatalytic Synthesis of 4-Aryl-1,2,3,4-tetrahydropyridines from Morita-Baylis-Hillman Carbonates through a One-Pot Three-Component Cyclization.

    Science.gov (United States)

    Wei, Jian; Li, Yuntong; Tao, Cheng; Wang, Huifei; Cheng, Bin; Zhai, Hongbin; Li, Yun

    2018-01-19

    An efficient DABCO-catalyzed three-component formal [3 + 2 + 1] annulation, involving a Morita-Baylis-Hillman carbonate, a 1,3-ketoester, and a primary amine, leading to one-pot synthesis of substituted 4-aryl-1,2,3,4-tetrahydropyridines, has been developed. The densely functionalized products were generally obtained in good to excellent yields under mild conditions. The structures including the relative stereoconfigurations of the representative products were confirmed by X-ray diffraction analysis.

  8. Sequential polymerization of ethylene oxide, ε-caprolactone and l-lactide: A one-pot metal-free route to tri- and pentablock terpolymers

    KAUST Repository

    Zhao, Junpeng

    2014-01-01

    Metal-free polymerization of ethylene oxide (EO) catalyzed by a relatively mild phosphazene base (t-BuP2) was proven feasible, which enabled the one-pot sequential polymerization of EO, ε-caprolactone, and l-lactide. Using either 3-phenyl-1-propanol or water as an initiator, the corresponding triblock or pentablock terpolymers were easily prepared. © 2014 the Partner Organisations.

  9. KSF-supported heteropoly acids catalyzed one-pot synthesis of α ...

    African Journals Online (AJOL)

    In the presence of KSF-supported heteropoly acid as a heterogeneous, reusable and inexpensive catalyst, three-component reactions between aldehydes or ketones, amines, and trimethylsilyl cyanide preceded to afford α-aminonitriles in excellent yields, very short reaction times, and low loading of catalyst. This catalyst ...

  10. SnO 2 /SiO 2 Nanocomposite Catalyzed One-pot, Four-component ...

    African Journals Online (AJOL)

    -Amino-3-Cyanopyridines. ... (SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT–IR), Brunauer-Emmer-Teller (BET) surface area, and temperature-programmed desorption of ammonia (NH3-TPD).

  11. Potassium Hydroxide Impregnated Alumina (KOH-Alumina) as a Recyclable Catalyst for the Solvent-Free Multicomponent Synthesis of Highly Functionalized Substituted Pyridazines and/or Substituted Pyridazin-3(2H)-ones under Microwave Irradiation.

    Science.gov (United States)

    Mecadon, Hormi; Myrboh, Bekington

    2011-01-01

    The work described herein employs potassium hydroxide impregnated alumina (KOH-alumina) as a mild, efficient, and recyclable catalyst for a one-pot solvent-free and environmentally safer synthesis of 3,4,6-triarylpyridazines and some substituted pyridazines from active methylene carbonyl species, 1,2-dicarbonyls, and hydrazine hydrate by microwave (MW) irradiation. The method offers highly convergent, inexpensive, and functionality-tolerable procedure for rapid access to important pyridazine compounds in good yields.

  12. Bis (imino) pyridine (BIMP) Fe (II) catalyses one-pot green ...

    Indian Academy of Sciences (India)

    pyridine (BIMP) Fe(II) catalyses one-pot green condensation of resorcinol, malononitrile, aromatic aldehydes and cyclohexanone. Saman Damavandi Reza Sandaroos. Volume 124 Issue 2 March 2012 pp 483-486 ...

  13. One-pot desymmetrizing hydroformylation/carbonyl ene cyclization process: straightforward access to highly functionalized cyclohexanols.

    Science.gov (United States)

    Bigot, Aurélien; Breuninger, Daniel; Breit, Bernhard

    2008-12-04

    Rapid access to highly functionalized alkylidene cyclohexanols through a one-pot desymmetrizing hydroformylation/carbonyl ene cyclization starting from simple bisalkenylcarbinols is reported. Mechanistic insight into the carbonyl ene reaction is given, highlighting the importance of hyperconjugative substituent effects.

  14. T3P as an efficient cyclodehydration reagent for the one-pot ...

    Indian Academy of Sciences (India)

    Abstract. A scalable and environmentally friendly one-pot method for the synthesis of 2-amino-1,3,4-oxadiazoles from acylhydrazides and isocyanates has been achieved with propane phosponic anhydride (T3P) acting as cyclodehydrating reagent.

  15. Boric acid as a mild and efficient catalyst for one-pot synthesis of 1 ...

    Indian Academy of Sciences (India)

    amidoalkyl-2- naphthol derivatives via a one-pot three-component condensation of 2-naphthol, aldehydes and amide in the presence of boric acid as a mild catalyst. Keywords. Multicomponent reaction; amidoalkyl naphthol; boric acid; catalyst; ...

  16. Structural Transitions of Solvent-Free Oligomer-Grafted Nanoparticles

    KAUST Repository

    Chremos, Alexandros

    2011-09-01

    Novel structural transitions of solvent-free oligomer-grafted nanoparticles are investigated by using molecular dynamics simulations of a coarse-grained bead-spring model. Variations in core size and grafting density lead to self-assembly of the nanoparticles into a variety of distinct structures. At the boundaries between different structures, the nanoparticle systems undergo thermoreversible transitions. This structural behavior, which has not been previously reported, deviates significantly from that of simple liquids. The reversible nature of these transitions in solvent-free conditions offers new ways to control self-assembly of nanoparticles at experimentally accessible conditions. © 2011 American Physical Society.

  17. Organic Synthesis under Solvent-free Condition. An Environmentally ...

    Indian Academy of Sciences (India)

    GENERAL I ARTICLE. Organic Synthesis under Solvent-free Condition. An Environmentally Benign Procedure - II. The author is a Professor of Organic Chemistry at. Bangalore University,. Bangalore. His main area of research is organosilicon chemistry with particular attention to developing new synthetic procedures and.

  18. Highly Efficient Method for Solvent-Free Synthesis of Diarylmethane ...

    African Journals Online (AJOL)

    NICO

    2011-02-25

    Feb 25, 2011 ... methane and triarylmethane was studied at room temperature, under solvent-free conditions, for five successive runs. In each run, the reaction was stopped after 120 min, cooled and sus- pended in anhydrous CH2Cl2. The suspension was then filtered and the reagent washed with anhydrous CH2Cl2 (2 ...

  19. dichlorodiazene dioxides using levulinic acid under solvent-free ...

    Indian Academy of Sciences (India)

    Administrator

    preparation of these compounds starting from alkenes adopting the Green Chemistry principle of solvent- free reaction. The procedure involves addition of NOCl generated in situ by the reaction of AcOH–HCl. (3 :1) with amyl nitrite to alkenes and treating the α-chloronitroso compounds obtained as dimers with levulinic acid ...

  20. Microwave accelerated solvent-free synthesis of flavanones

    Energy Technology Data Exchange (ETDEWEB)

    Sagrera, Gabriel J. [Universidad de la Republica, Montevideo (Uruguay). Facultad de Ciencias. Dept. de Quimica Organica]. E-mail: gseoane@fq.edu.uy; Seoane, Gustavo A. [Universidad de la Republica, Montevideo (Uruguay). Facultad de Quimica

    2005-07-15

    Microwave irradiation of chalcones under solvent-free conditions resulted in a 'green-chemistry' procedure for the preparation of flavanones in very good yields. Using an unmodified household microwave oven, different mineral supports and catalysts were tested. By irradiation of chalcones with 30% TFA over silica gel, eleven known flavanones and five new compounds were prepared in high yields. (author)

  1. Solvent-free synthesis of xanthene derivatives by Preyssler type ...

    African Journals Online (AJOL)

    naphthol in the presence of a catalytic amount of Preyssler type heteropolyacid, H14[NaP5W30O110], as a green and reusable catalyst under solvent-free conditions to form a variety of new xanthene derivatives in very good yields.

  2. Highly efficient solvent-free synthesis of pyranopyrazoles by a ...

    Indian Academy of Sciences (India)

    phate [(CH2)4SO3HMIM][HSO4], an acidic ionic liquid and as a catalyst, under solvent-free conditions. The ... cyano ethylene. In addition, weak bases can also be used for this Michael-type cyclization.7 Other recent methods for the synthesis of pyranopyrazoles ... absolute ethanol,8 a two-component reaction involv-.

  3. GRINDING SOLVENT-FREE PAAL-KNORR PYRROLE SYNTHESIS ...

    African Journals Online (AJOL)

    solvent-free condensation reaction of 2,5-hexanedione with various primary amines (Paal-Knorr pyrrole synthesis) on smectite ... Paal-Knorr pyrrole synthesis on smectites as recyclable and green catalysts. Bull. Chem. Soc. ..... 10. a) Determined in our laboratory by temperature-programmed desorption of ammonia gas.

  4. Organic Synthesis under Solvent-free Condition. An Environmentally ...

    Indian Academy of Sciences (India)

    with particular attention to developing new synthetic procedures and reagents, and ... academic interest in solid-solid reactions have led them in recent times to develop methodologies for solvent-free ... ronment-friendly synthetic procedures has made them turn their attention to minimize or circumvent the use of solvents.

  5. Highly efficient solvent-free synthesis of pyranopyrazoles by a ...

    Indian Academy of Sciences (India)

    organic synthesis and medicinal chemistry because they are one-pot processes bringing together three or more components and show high atom economy and high selectivity.1,2 MCRs have great contribution in con- vergent synthesis of complex and important organic molecules from simple and readily available starting.

  6. A Solvent-free Synthesis of Polyhydroquinolines via Hantzsch ...

    African Journals Online (AJOL)

    A simple and efficient procedure for the synthesis of polyhydroquinolines was developed, involving a one-pot four-component Hantzsch condensation of aromatic aldehydes, 1,3-cyclohexanediones, alkyl acetoacetate and ammonium acetate in the presence of a catalytic amount of nanomagnetic-supported sulfonic acid ...

  7. One-pot, mix-and-read peptide-MHC tetramers

    DEFF Research Database (Denmark)

    Leisner, Christian Valdemar Vinge; Loeth, Nina; Lamberth, Kasper

    2008-01-01

    BACKGROUND: Cytotoxic T Lymphocytes (CTL) recognize complexes of peptide ligands and Major Histocompatibility Complex (MHC) class I molecules presented at the surface of Antigen Presenting Cells (APC). Detection and isolation of CTL's are of importance for research on CTL immunity, and development...... molecules can be refolded in vitro, tetramerized with streptavidin, and used for specific T cell staining-all in a one-pot reaction without any intervening purification steps. CONCLUSIONS/SIGNIFICANCE: We have developed an efficient "one-pot, mix-and-read" strategy for peptide-MHC tetramer generation...

  8. KHSO 4 -catalyzed Three-component Synthesis of α

    African Journals Online (AJOL)

    Asimple, convenient and general method has been developed for the synthesis of-aminonitriles by a one-pot three-component condensation of aldehydes, amines and trimethyl silyl cyanide under solvent-free conditions in the presence of a catalytic amount of KHSO4 in good yields. The new method compares well in terms ...

  9. A novel polymeric catalyst for the one-pot synthesis of 2,4,5-triaryl ...

    Indian Academy of Sciences (India)

    Abstract. An efficient synthesis of 2,4,5-trisubstituted imidazoles is achieved by three component cyclo- condensation of benzil or benzoin, aldehyde and ammonium acetate by using novel polymeric catalyst. [poly(AMPS-co-AA)] under solvent-free conditions. The key advantages of this process are high yields, shorter.

  10. One-pot efficient green synthesis of 1, 4-dihydro-quinoxaline-2, 3 ...

    Indian Academy of Sciences (India)

    http://www.ias.ac.in/article/fulltext/jcsc/118/05/0425-0428. Keywords. Green chemistry; quinoxaline; o-phenylene diamine; oxalic acid; grinding; atom economy. ... temperature from substituted -phenylene diamine and oxalic acid under solvent-free conditions by a simple grinding method with unsurpassed atom economy.

  11. Boric acid as a mild and efficient catalyst for one-pot synthesis of 1 ...

    Indian Academy of Sciences (India)

    Multicomponent reaction; amidoalkyl naphthol; boric acid; catalyst; solvent-free synthesis. 1. Introduction. Multicomponent reactions (MCRs), in ... silica-sodium hydrogen sul- phate,14 molybdophosphoric acid (H3[P(Mo3O10)4]),15 ... The solid obtained was collected by filtration and purified by recrystallization from ethanol.

  12. Silica sulfuric acid promoted one-pot synthesis of benzo[4,5]imidazo ...

    African Journals Online (AJOL)

    A simple and efficient synthesis of benzo[4,5]imidazo[1,2-a]pyrimidine derivatives has been accomplished by the reaction of 2-aminobenzimidazole, aldehydes and β-dicarbonyl compounds under solvent-free conditions in the presence of silica sulfuric acid. KEY WORDS: Benzo[4,5]imidazo[1,2-a]pyrimidine, Silica sulfuric ...

  13. One-Pot Functionalization of Graphene with Porphyrin through Cycloaddition Reactions

    NARCIS (Netherlands)

    Zhang, Xiaoyan; Hou, Lili; Cnossen, Arjen; Coleman, Anthony C.; Ivashenko, Oleksii; Rudolf, Petra; Wees, Bart J. van; Browne, Wesley R.; Feringa, Ben L.

    Two types of graphene-based hybrid materials, graphene-TPP (TPP=tetraphenylporphyrin) and graphene-PdTPP (PdTPP=palladium tetraphenylporphyrin), were prepared directly from pristine graphene through one-pot cycloaddition reactions. The hybrid materials were characterized by thermogravimetric

  14. One-pot synthesis and UV-Visible absorption studies of novel ...

    Indian Academy of Sciences (India)

    One-pot synthesis and UV-Visible absorption studies of novel tricyclic heterocycle tethered Xanthene-1,8- ... Further, UV-Visible absorption properties of all the synthesized compounds were investigated in CHCl3, THF and ..... using JASCO UV-Visible absorption spectrophotometer in dilute solutions of chloroform at a.

  15. Two-Step, One-Pot Synthesis of Visible-Light-Responsive 6-Azopurines

    NARCIS (Netherlands)

    Kolarski, Dusan; Szymanski, Wiktor; Feringa, Ben L.

    2017-01-01

    The first general two-step, one-pot syntheticroute to 6-azopurines is presented. Microwave-assistednucleophilic aromatic substitution of protected 6-chloropurineswith hydrazines or hydrazides, followed by metal-free oxidationwith oxygen, gives 6-azopurines in high to excellent yields.Photophysical

  16. One-Pot Conversion of Carbohydrates into Furan Derivatives via Furfural and 5-Hydroxylmethylfurfural as Intermediates.

    Science.gov (United States)

    Liu, Bing; Zhang, Zehui

    2016-08-23

    Recently, there has been growing interest in the transformation of renewable biomass into value-added fuels and chemicals. The catalytic conversion of naturally abundant carbohydrates can generate two-important furan chemicals: 5-hydroxymethylfurfural (HMF) from C6 carbohydrates and furfural from C5 carbohydrates. Both HMF and furfural have received great interest as precursors in the synthesis of commodity chemicals and liquid fuels. In recent years, a trend has emerged to integrate sequential catalytic processes involving multistep reactions for the direct one-pot transformation of carbohydrates into the aimed fuels and chemicals. One-pot reactions have remarkably unique and environmentally friendly benefits, including the fact that isolation and purification of intermediate compounds can be avoided. Herein, the present article aims to review recent advances in the one-pot conversion of carbohydrates into furan derivatives via furfural and HMF as intermediates. Special attention will be paid to the catalytic systems, mechanistic insight, reaction pathways, and catalyst stability. It is expected that this review will guide researchers to develop effective catalytic systems for the one-pot transformation of carbohydrates into furan derivatives. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Diastereoselective one pot five-component reaction toward 4-(tetrazole)-1,3-oxazinanes

    NARCIS (Netherlands)

    Chandgude, Ajay L.; Narducci, Daniele; Kurpiewska, Katarzyna; Kalinowska-Tluscik, Justyna; Domling, Alexander

    2017-01-01

    A diastereoselective one pot five-component reaction toward the synthesis of 4-(tetrazole)-1,3-oxazinanes has been reported. The sonication-accelerated, catalyst-free, simple, general and highly time efficient, Asinger-Ugi-tetrazole reaction was used for the synthesis of diverse

  18. One-pot synthesis of an Mn(III)–Cu(II)–Mn(III) trinuclear ...

    Indian Academy of Sciences (India)

    Keywords. One-pot synthesis; trinuclear heterometallic compound; crystal structure; dithiolene; non- .... elemental analysis, ESR, IR and electronic spectral studies. Compound 1 was finally characterized un- ambiguously by single crystal X-ray structural analysis. Table 1. .... sulphur involving interaction with Mn(III) cation).

  19. Gene assembly via one-pot chemical ligation of DNA promoted by DNA nanostructures

    DEFF Research Database (Denmark)

    Manuguerra, Ilenia; Croce, Stefano; El-Sagheer, Afaf H.

    2018-01-01

    Current gene synthesis methods are driven by enzymatic reactions. Here we report the one-pot synthesis of a chemically-ligated gene from 14 oligonucleotides. The chemical ligation benefits from the highly efficient click chemistry approach templated by DNA nanostructures, and produces modified DNA...

  20. Boric acid as a mild and efficient catalyst for one-pot synthesis of 1 ...

    Indian Academy of Sciences (India)

    Abstract. An efficient green chemistry method has been developed for the synthesis of 1-amidoalkyl-2-naphthol derivatives via a one-pot three-component condensation of 2-naphthol, aldehydes and amide in the presence of boric acid as a mild catalyst.

  1. Bis(imino)pyridine (BIMP) Fe(II) catalyses one-pot green ...

    Indian Academy of Sciences (India)

    483–486. c Indian Academy of Sciences. Bis(imino)pyridine (BIMP) Fe(II) catalyses one-pot green condensation of resorcinol, malononitrile, aromatic aldehydes and cyclohexanone. SAMAN DAMAVANDIa,∗ and REZA SANDAROOSb. aDepartment of Chemistry, Sarvestan Branch, Islamic Azad University, Sarvestan, Iran.

  2. Boric acid as a mild and efficient catalyst for one-pot synthesis of 1

    Indian Academy of Sciences (India)

    Abstract. An efficient green chemistry method has been developed for the synthesis of 1-amidoalkyl-2-naphthol derivatives via a one-pot three-component condensation of 2-naphthol, aldehydes and amide in the presence of boric acid as a mild catalyst.

  3. One-Pot, Simple and Efficient Synthesis of Triaryl-1H-imidazoles by ...

    African Journals Online (AJOL)

    2,4,5-Triarylimidazoles have been obtained in excellent yields by the one-pot three-component condensation of bis-aryl α-hydroxyketones, aromatic aldehydes and ammonium acetate by the action of inexpensive, readily available and nontoxic KMnO4/CuSO4 under mild reaction conditions. The present method is simple, ...

  4. Ammonia-Promoted One-Pot Tetrazolopiperidinone Synthesis by Ugi Reaction

    NARCIS (Netherlands)

    Patil, Pravin; Kurpiewska, Katarzyna; Kalinowska-Tłuścik, Justyna; Dömling, Alexander

    2017-01-01

    Ammonia in the tetrazole Ugi variation together with α-amino acid methyl ester-derived isocyanides provides tetrazolopiperidinones in good to high yields in one pot. The scope and limitations of this reaction were investigated by performing >70 reactions. The scaffold is useful to fill

  5. Ammonia-Promoted One-Pot Tetrazolopiperidinone Synthesis by Ugi Reaction.

    Science.gov (United States)

    Patil, Pravin; Kurpiewska, Katarzyna; Kalinowska-Tłuścik, Justyna; Dömling, Alexander

    2017-05-08

    Ammonia in the tetrazole Ugi variation together with α-amino acid methyl ester-derived isocyanides provides tetrazolopiperidinones in good to high yields in one pot. The scope and limitations of this reaction were investigated by performing >70 reactions. The scaffold is useful to fill high-throughput screening decks and in structure-based drug design.

  6. Water mediated eco-friendly green protocol for one-pot synthesis of ...

    Indian Academy of Sciences (India)

    793–799. c Indian Academy of Sciences. Water mediated eco-friendly green protocol for one-pot synthesis of α-aminophosphonates at ambient conditions. SANTHOSH REDDY MANDHA, MANJULA ALLA. ∗ and VITTAL RAO BOMMENA. Crop Protection Chemicals, CSIR-Indian Institute of Chemical Technology, Tarnaka,.

  7. Silica-supported ionic liquid as highly efficient catalyst for one-pot ...

    Indian Academy of Sciences (India)

    supported ionic liquid as highly efficient catalyst for one-pot synthesis of acenaphtho[1,2-b]furan compounds. REZA SANDAROOSa,∗, MOHAMMAD TAGHI GOLDANIb,∗ and SAMAN DAMAVANDIc. aDepartment of Chemistry, Faculty of Science, ...

  8. A new one-pot synthesis of 1,2,4-oxadiazoles from aryl nitriles ...

    Indian Academy of Sciences (India)

    Scheme 1. One-pot synthesis of 1,2,4-oxadiazole derivatives. in potassium bromide pellets on a FT-IR Bruker Tensor. 27 over the range 400–4000cm. −1 . Elemental analysis performed by a Perkin Elmer 2004 (II) CHN Analyzer. Melting points were measured with an Elec- trothermal Engineering LTD 9200 apparatus. Gas.

  9. One pot direct synthesis of amides or oxazolines from carboxylic acids using Deoxo-Fluor reagent.

    Science.gov (United States)

    Kangani, Cyrous O; Kelley, David E

    2005-12-19

    A mild and highly efficient one pot-one step condensation and/or condensation-cyclization of various acids to amides and/or oxazolines using Deoxo-Fluor reagents is described. Parallel syntheses of various free fatty acids with 2-amino-2, 2-dimethyl-1-propanol resulted with excellent yields.

  10. One-pot synthesis of 2,5-dihydropyrroles from terminal alkynes, azides, and propargylic alcohols by relay actions of copper, rhodium, and gold.

    Science.gov (United States)

    Miura, Tomoya; Tanaka, Takamasa; Matsumoto, Kohei; Murakami, Masahiro

    2014-12-01

    Relay actions of copper, rhodium, and gold formulate a one-pot multistep pathway, which directly gives 2,5-dihydropyrroles starting from terminal alkynes, sulfonyl azides, and propargylic alcohols. Initially, copper-catalyzed 1,3-dipolar cycloaddition of terminal alkynes with sulfonyl azides affords 1-sulfonyl-1,2,3-triazoles, which then react with propargylic alcohols under the catalysis of rhodium. The resulting alkenyl propargyl ethers subsequently undergo the thermal Claisen rearrangement to give α-allenyl-α-amino ketones. Finally, a gold catalyst prompts 5-endo cyclization to produce 2,5-dihydropyrroles. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. An efficient synthesis of β-amino ketone compounds through one-pot three-component Mannich-type reactions using bismuth nitrate as catalyst

    Directory of Open Access Journals (Sweden)

    S. Sheik Mansoor

    2015-07-01

    Full Text Available Three components one-pot Mannich reaction of aromatic ketone, aromatic aldehyde and aromatic amines has been efficiently catalyzed by recyclable bismuth nitrate (Bi(NO33, BN at ambient temperature to give various β-amino carbonyl compounds in high yields. This method has advantages of mild condition, no environmental pollution, and simple work-up procedures. Most importantly, β-amino carbonyl compounds with ortho-substituted aromatic amines are obtained in acceptable to moderate yields by this methodology.

  12. One-Pot Synthesis of N-(α-Peroxy)Indole/Carbazole via Chemoselective Three-Component Condensation Reaction in Open Atmosphere

    KAUST Repository

    Wang, Xinbo

    2015-11-06

    A facile one-pot synthesis of N-(α-peroxy)indole and N-(α-peroxy)carbazole has been developed using metal-free, organo-acid-catalyzed three-component condensation reactions of indole/carbazole, aldehyde, and peroxide. Based on the reaction discovered, a new synthetic proposal for Fumitremorgin A and Verruculogen is introduced. Such a protocol could be easily handled and scaled up in an open atmosphere with a wide substrate scope, enabling the construction of a new molecule library.

  13. An N-Heterocyclic Carbene-Mediated, Enantioselective and Multicatalytic Strategy to Access Dihydropyranones in a Sequential Three-Component One-Pot Reaction.

    Science.gov (United States)

    Fuchs, Patrick J W; Zeitler, Kirsten

    2017-11-17

    The multicatalytic generation of 3,5,6-trisubstituted 3,4-dihydropyranones with high enantioselectivity using a highly convergent strategy starting from commercially available precursors is reported. The operationally simple three-step, one-pot protocol merges H-bond and NHC catalysis to provide crucial, reactive β-unsubstituted enones from nitroalkenes as latent 1,2-biselectrophiles. These intermediates are directly funneled into a further NHC-catalyzed formal hetero-Diels-Alder reaction to deliver manifold chiral C(4)-unsubstituted dihydropyranones (typical ee >98%), allowing aliphatic and heteroaromatic substituents and hence expanding the scope of this Michael addition/lactonization.

  14. 21 CFR 182.20 - Essential oils, oleoresins (solvent-free), and natural extractives (including distillates).

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Essential oils, oleoresins (solvent-free), and...) SUBSTANCES GENERALLY RECOGNIZED AS SAFE General Provisions § 182.20 Essential oils, oleoresins (solvent-free), and natural extractives (including distillates). Essential oils, oleoresins (solvent-free), and...

  15. 21 CFR 582.20 - Essential oils, oleoresins (solvent-free), and natural extractives (including distillates).

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Essential oils, oleoresins (solvent-free), and... SUBSTANCES GENERALLY RECOGNIZED AS SAFE General Provisions § 582.20 Essential oils, oleoresins (solvent-free), and natural extractives (including distillates). Essential oils, oleoresins (solvent-free), and...

  16. Solvent-Free Synthesis of Some1-Acetyl Pyrazoles

    Energy Technology Data Exchange (ETDEWEB)

    Thirunarayanan, Ganesamoorthy [Annamalai Univ., Tamil Nadu (India); Sekar, Krishnamoorthy Guna [National College, Tiruchirappalli (India)

    2013-10-15

    Some N-acetyl pyrazoles including 1-(3-(3,4-dichlorophenyl)-5-(substituted phenyl)-4,5-dihydro-{sup 1}H-pyrazole-1-yl) ethanones have been synthesised by solvent free cyclization cum acetylation of chalcones like substituted styryl 3,4-dichlorophenyl ketones using hydrazine hydrate and acetic anhydride in presence of catalytic amount of fly-ash: H{sub 2}SO{sub 4} catalyst. The yield of these N-acetyl pyrazole derivatives are more than 75%. The synthesised N-acetyl pyrazoline derivatives were characterized by their physical constants and spectral data.

  17. Synthesis of halide- and solvent free metal borohydrides

    DEFF Research Database (Denmark)

    Grinderslev, Jakob; Møller, Kasper Trans; Richter, Bo

    have challenges due to their high desorption kinetics and limited reversibility at moderate conditions.[2],[3],[4] In this work, we present a new approach to synthesize halide- and solvent free metal borohydrides starting from the respective metal hydride. The synthetic strategy ensures that no metal...... to the metal. Hence, the powdered M(BH4)3∙DMS is heated to 140 °C for 4 hours to obtain pure M(BH4)3. The rare-earth metal borohydrides have been investigated by infrared spectroscopy and thermal analysis (TGA-DSC-MS). Furthermore, the structural trends are investigated by synchrotron radiation powder X...

  18. Solvent-free synthesis, spectral correlations and antimicrobial activities of some aryl E 2-propen-1-ones

    Science.gov (United States)

    Sathiyamoorthi, K.; Mala, V.; Sakthinathan, S. P.; Kamalakkannan, D.; Suresh, R.; Vanangamudi, G.; Thirunarayanan, G.

    2013-08-01

    Totally 38 aryl E 2-propen-1-ones including nine substituted styryl 4-iodophenyl ketones have been synthesised using solvent-free SiO2-H3PO4 catalyzed Aldol condensation between respective methyl ketones and substituted benzaldehydes under microwave irradiation. The yields of the ketones are more than 80%. The synthesised chalcones were characterized by their analytical, physical and spectroscopic data. The spectral frequencies of synthesised substituted styryl 4-iodophenyl ketones have been correlated with Hammett substituent constants, F and R parameters using single and multi-linear regression analysis. The antimicrobial activities of 4-iodophenyl chalcones have been studied using Bauer-Kirby method.

  19. Gold-silver-alloy nanoprobes for one-pot multiplex DNA detection

    Energy Technology Data Exchange (ETDEWEB)

    Doria, G; Larguinho, M; Dias, J T; Baptista, P V [Centro de Investigacao em Genetica Molecular Humana (CIGMH), Departamento de Ciencias da Vida, Faculdade de Ciencias e Tecnologia, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal); Pereira, E [Rede de Quimica e Tecnologia (REQUIMTE), Departamento de Quimica, Faculdade de Ciencias, Universidade do Porto, 4169-007 Porto (Portugal); Franco, R, E-mail: pmvb@fct.unl.pt [Rede de Quimica e Tecnologia (REQUIMTE), Departamento de Quimica, Faculdade de Ciencias e Tecnologia, Universidade Nova de Lisboa, 2829-516 Caparica (Portugal)

    2010-06-25

    A specific colorimetric DNA detection method based on oligonucleotide functionalized gold-silver-alloy nanoparticles (AuAg-alloy-nanoprobes) is presented. The AuAg-alloy-nanoprobes were then used for the specific detection of a DNA sequence from TP53-a gene involved in cancer development. The AuAg-alloy-nanoprobes were then used in combination with Au-nanoprobes for a one-pot dual-colour detection strategy that allowed for the simultaneous differential detection of two distinct target sequences. This system poses an unprecedented opportunity to explore the combined use of metal nanoparticles with different composition towards the development of a multiplex one-pot colorimetric assay for DNA detection.

  20. Gold-silver-alloy nanoprobes for one-pot multiplex DNA detection

    International Nuclear Information System (INIS)

    Doria, G; Larguinho, M; Dias, J T; Baptista, P V; Pereira, E; Franco, R

    2010-01-01

    A specific colorimetric DNA detection method based on oligonucleotide functionalized gold-silver-alloy nanoparticles (AuAg-alloy-nanoprobes) is presented. The AuAg-alloy-nanoprobes were then used for the specific detection of a DNA sequence from TP53-a gene involved in cancer development. The AuAg-alloy-nanoprobes were then used in combination with Au-nanoprobes for a one-pot dual-colour detection strategy that allowed for the simultaneous differential detection of two distinct target sequences. This system poses an unprecedented opportunity to explore the combined use of metal nanoparticles with different composition towards the development of a multiplex one-pot colorimetric assay for DNA detection.

  1. One-pot synthesis of thermoplastic mixed paramylon esters using trifluoroacetic anhydride.

    Science.gov (United States)

    Shibakami, Motonari; Tsubouchi, Gen; Sohma, Mitsugu; Hayashi, Masahiro

    2015-03-30

    Mixed paramylon esters prepared from paramylon (a storage polysaccharide of Euglena), acetic acid, and a long-chain fatty acid by one-pot synthesis using trifluoroacetic anhydride as a promoter and solvent were shown to have thermoplasticity. Size exclusion chromatography indicated that the mixed paramylon esters had a weight average molecular weight of approximately 4.9-6.7×10(5). Thermal analysis showed that these esters were stable in terms of the glass transition temperature (>90°C) and 5% weight loss temperature (>320°C). The degree of substitution of the long alkyl chain group, a dominant factor determining thermoplasticity, was controlled by tuning the feed molar ratio of acetic acid and long-chain fatty acid to paramylon. These results implied that the one-pot synthesis is useful for preparing structurally-well defined thermoplastic mixed paramylon esters with high molecular weight. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Caryophyllene driven diversity in an one-pot rearrangement of oxidation and transanular reactions

    Science.gov (United States)

    Tang, Hao-Yu; Quan, Lu-Lu; Yu, Jie; Zhang, Qiang; Gao, Jin-Ming

    2018-03-01

    Diversity oriented synthesis starting from natural products is a newly coming strategy to build diverse skeletons to meet the demands of high throughput screening in drug development. Caryophyllene was being considered as an ideal starting point to build divers natural-like sesquiterpenes due to its rich sources and build-in reactivity. In this paper, six new natural-like products (2-7) were synthesized form the natural cryophyllene oxide via cascade oxidation and transannular reactions in a one-pot procedure. Their structures were elucidated by exhaustive spectra method including 2D NMR and X-ray diffraction. Of the products, compounds 6 and 7 possess very similar skeleton to natural products. Our findings demonstrated that one-pot cascade reactions on macrocyclic natural products is a concise strategy to create diverse natural-like skeletons.

  3. A one-pot radiosynthesis of [125I]iodoazido photoaffinity labels

    International Nuclear Information System (INIS)

    Wilson, A.A.; Dannals, R.F.; Ravert, H.T.; Wagner, H.N. Jr.; Grigoriadis, D.E.

    1989-01-01

    A useful method for preparing radioiodinated photoaffinity labels from alkyl anilines which offer significant advantages over present methods is described. The one-pot synthesis gives good radiochemical yields (40-64%) of pure, high specific activity (350-1500 mCi/μmol) 124 I labelled iodaryl azides while minimising manipulation of radioactive materials. Purification of the [ 125 I]iodoazido photoaffinity labels is achieved by high performance liquid chromatography. (author)

  4. A Tractable and Efficient One-Pot Synthesis of 5'-Azido-5'-deoxyribonucleosides

    Directory of Open Access Journals (Sweden)

    Theodore V. Peterson

    2014-02-01

    Full Text Available Synthetic routes to 5'-azidoribonucleosides are reported for adenosine, cytidine, guanosine, and uridine, resulting in a widely applicable one-pot methodology for the synthesis of these and related compounds. The target compounds are appropriate as precursors in a variety of purposive syntheses, as the synthetic and therapeutic relevance of azido- and amino-modified nucleosides is expansive. Furthermore, in the conversion of alcohols to azides, these methods offer a tractable alternative to the Mitsunobu and other more difficult reactions.

  5. One-Pot Syntesis of 3-Functionalized 4-Hydroxycoumarin under Catalyst-Free Conditions

    Directory of Open Access Journals (Sweden)

    Yang Gao

    2018-01-01

    Full Text Available A concise and efficient one-pot synthesis of 3-functionalized 4-hydroxycoumarin derivatives via a three-component domino reaction of 4-hydroxycoumarin, phenylglyoxal and 3-arylaminocyclopent-2-enone or 4-arylaminofuran-2(5H-one under catalyst-free and microwave irradiation conditions is described. This synthesis involves a group-assisted purification process, which avoids traditional recrystallization and chromatographic purification methods.

  6. Asymmetric Formation of Bridged Benzoxazocines through an Organocatalytic Multicomponent Dienamine-Mediated One-Pot Cascade

    DEFF Research Database (Denmark)

    Ransborg, Lars Krogager; Overgaard, Mette Kiilerich; Hejmanowska, Joanna

    2014-01-01

    An organocatalytic one-pot cascade leading to the stereoselective formation of novel bridged benzoxazocines is presented. The developed methodology is based on the first example of a γ-selective-Mannich-initiated cascade reaction and allows for direct annulation of the bridged benzoxazocines...... by incorporation of various α,β-unsaturated aldehydes, electron-rich anilines, and electron-deficient salicylaldehydes. The synthetic applicability of the products is demonstrated by relevant transformations....

  7. One-pot polyol synthesis of highly monodisperse short green silver nanorods.

    Science.gov (United States)

    Patarroyo, Javier; Genç, Aziz; Arbiol, Jordi; Bastús, Neus G; Puntes, Victor

    2016-09-21

    Green silver nanorods (Ag NRs) of a low aspect ratio (2.8) have been produced in high yields via an optimized, simple, and robust one-pot polyol method in the presence of tannic acid, which favors the nucleation of decahedral seeds needed for the production of monodisperse Ag NRs. These Ag NRs were further used as sacrificial templates to produce Au hollow nanostructures via galvanic replacement reaction with HAuCl4 at room temperature.

  8. An Efficient One-Pot Multicomponent Synthesis of 4-Aza-Podophyllotoxin Derivatives in Ionic Liquid

    Directory of Open Access Journals (Sweden)

    Hossein Naeimi

    2013-01-01

    Full Text Available A simple, green, and efficient procedure for the synthesis of 4-aza-podophyllotoxin derivatives by using a one-pot three-component reaction of benzaldehydes, 1,3-cyclohexanediones, and anilinolactones in the presence of catalytic amount of alum in 1-butyl-3-methylimidazolium triflate as green media is described. This reaction proceeded under mild conditions with the use of an inexpensive and readily available catalyst, high to excellent yields, and simple workup procedure.

  9. Facile one-pot synthesis of porphyrin based porous polymer networks (PPNs) as biomimetic catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Zou, LF; Feng, DW; Liu, TF; Chen, YP; Fordham, S; Yuan, S; Tian, J; Zhou, HC

    2015-01-01

    Stable porphyrin based porous polymer networks, PPN-23 and PPN-24, have been synthesized through a facile one-pot approach by the aromatic substitution reactions of pyrrole and aldehydes. PPN-24(Fe) shows high catalytic efficiency as a biomimetic catalyst in the oxidation reaction of 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) in the presence of H2O2.

  10. An efficient catalytic reductive amination: A facile one-pot access to ...

    Indian Academy of Sciences (India)

    Vol. 127, No. 4, April 2015, pp. 711–716. c Indian Academy of Sciences. DOI 10.1007/s12039-015-0825-y. An efficient catalytic reductive amination: A facile one-pot ..... 68 55. 4. (a) Hiroi R, Miyoshi N and Wada M 2002 Chem. Lett. 31. 274; (b) Suwa T, Shibata I, Nishino K and Baba A 1999. Org. Lett. 1 1579; (c) Shibata I, ...

  11. Imides: forgotten players in the Ugi reaction. One-pot multicomponent synthesis of quinazolinones.

    Science.gov (United States)

    Mossetti, Riccardo; Pirali, Tracey; Saggiorato, Dèsirèe; Tron, Gian Cesare

    2011-06-28

    Up to now, the synthesis of quinazolinones has required lengthy synthetic procedures. Here, we describe an innovative one-pot multicomponent reaction leading to highly substituted quinazolinones. We believe that this novel transformation may open the door for the generation of new and pharmacologically active quinazolinones, but, most important of all, the resurrection of the imide-Ugi scaffold paves the way for the synthesis of novel molecular architectures. This journal is © The Royal Society of Chemistry 2011

  12. The development of a one-pot 1,4-addition/nitro-Mannich reaction

    OpenAIRE

    Mills, M. R.

    2010-01-01

    The introduction of this thesis reviews the three areas of importance to the research carried out. These are the nitro-Mannich reaction, the conjugate addition of nucleophiles to nitro-alkenes and the diastereoselectivity of electrophilic additions to substrates bearing an α-stereocentre. The Results and Discussion details the research carried out into the development of a one-pot 1,4-addition/nitro-Mannich reaction. Initially the research focused on triggering the reaction ...

  13. Recent Advances in the Catalytic One-Pot Synthesis of Flavonoids and Chromones.

    Science.gov (United States)

    Mohadeszadeh, Manijeh; Iranshahi, Mehrdad

    2017-01-01

    Flavonoids and chromones are two important classes of natural products that have various biological properties. During the past 10 years, there has been a significant increase in studies on the one-pot synthesis of flavonoids and chromones as medicinal scaffolds in drug discovery. This review describes the scope, mechanistic properties and regio- and chemo-selectivity features of several recently developed one-pot procedures for the synthesis of substituted chromones and flavonoids that have recently been published. Special importance is placed on the most promising and exciting medicinal applications of flavonoids and chromones. In this review, we discuss the progress on the synthesis of flavonoid and chromone derivatives in the presence of metal catalysts, organocatalysts, solid surfaces, microwave irradiation, acid and base catalysis, etc. For example, flavones can be prepared via the catalytic coordination of palladium complexes in a short time and at a low temperature with a high yield. Additionally, the one-pot synthesis of 2-substituted chromones via metal triflate (Yb(OTf)3) has provided the best result for this type of reaction with a high yield and a high regio and chemoselectivity. Generally, this review proposes the first specific overview of this developing and rapidly expanding field of flavonoid synthesis. We also discuss the mechanisms and advantages and disadvantages of methods for the synthesis of flavonoids and chromones. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  14. One-pot enzymatic conversion of carbon dioxide and utilization for improved microbial growth.

    Science.gov (United States)

    Hong, Sung-Gil; Jeon, Hancheol; Kim, Han Sol; Jun, Seung-Hyun; Jin, EonSeon; Kim, Jungbae

    2015-04-07

    We developed a process for one-pot CO2 conversion and utilization based on simple conversion of CO2 to bicarbonate at ambient temperature with no energy input, by using the cross-linking-based composites of carboxylated polyaniline nanofibers (cPANFs) and carbonic anhydrase. Carbonic anhydrase was immobilized on cPANFs via the approach of magnetically separable enzyme precipitate coatings (Mag-EPC), which consists of covalent enzyme attachment, enzyme precipitation, and cross-linking with amine-functionalized magnetic nanoparticles. Mag-EPC showed a half-life of 236 days under shaking, even resistance to 70% ethanol sterilization, and recyclability via facile magnetic separation. For one-pot CO2 conversion and utilization, Mag-EPC was used to accelerate the growth of microalga by supplying bicarbonate from CO2, representing 1.8-fold increase of cell concentration when compared to the control sample. After two repeated uses via simple magnetic separation, the cell concentration with Mag-EPC was maintained as high as the first cycle. This one-pot CO2 conversion and utilization is an alternative as well as complementary process to adsorption-based CO2 capture and storage as an environmentally friendly approach, demanding no energy input based on the effective action of the stabilized enzyme system.

  15. Solvent-free Liquid Crystals and Liquids from DNA.

    Science.gov (United States)

    Liu, Kai; Shuai, Min; Chen, Dong; Tuchband, Michael; Gerasimov, Jennifer Y; Su, Juanjuan; Liu, Qing; Zajaczkowski, Wojciech; Pisula, Wojciech; Müllen, Klaus; Clark, Noel A; Herrmann, Andreas

    2015-03-23

    As DNA exhibits persistent structures with dimensions that exceed the range of their intermolecular forces, solid-state DNA undergoes thermal degradation at elevated temperatures. Therefore, the realization of solvent-free DNA fluids, including liquid crystals and liquids, still remains a significant challenge. To address this intriguing issue, we demonstrate that combining DNA with suitable cationic surfactants, followed by dehydration, can be a simple generic scheme for producing these solvent-free DNA fluid systems. In the anhydrous smectic liquid crystalline phase, DNA sublayers are intercalated between aliphatic hydrocarbon sublayers. The lengths of the DNA and surfactant are found to be extremely important in tuning the physical properties of the fluids. Stable liquid-crystalline and liquid phases are obtained in the -20 °C to 200 °C temperature range without thermal degradation of the DNA. Thus, a new type of DNA-based soft biomaterial has been achieved, which will promote the study and application of DNA in a much broader context. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Photo-triggered solvent-free metamorphosis of polymeric materials.

    Science.gov (United States)

    Honda, Satoshi; Toyota, Taro

    2017-09-11

    Liquefaction and solidification of materials are the most fundamental changes observed during thermal phase transitions, yet the design of organic and polymeric soft materials showing isothermal reversible liquid-nonliquid conversion remains challenging. Here, we demonstrate that solvent-free repeatable molecular architectural transformation between liquid-star and nonliquid-network polymers that relies on cleavage and reformation of a covalent bond in hexaarylbiimidazole. Liquid four-armed star-shaped poly(n-butyl acrylate) and poly(dimethyl siloxane) with 2,4,5-triphenylimidazole end groups were first synthesized. Subsequent oxidation of the 2,4,5-triphenylimidazoles into 2,4,5-triphenylimidazoryl radicals and their coupling with these liquid star polymers to form hexaarylbiimidazoles afforded the corresponding nonliquid network polymers. The resulting nonliquid network polymers liquefied upon UV irradiation and produced liquid star-shaped polymers with 2,4,5-triphenylimidazoryl radical end groups that reverted to nonliquid network polymers again by recoupling of the generated 2,4,5-triphenylimidazoryl radicals immediately after terminating UV irradiation.The design of organic and polymeric soft materials showing isothermal reversible liquid-nonliquid conversion is challenging. Here, the authors show solvent-free repeatable molecular architectural transformation between liquid-star and non-liquid-network polymers by the cleavage and reformation of covalent bonds in the polymer chain.

  17. A facile one-pot green synthesis and antibacterial activity of 2-amino-4H-pyrans and 2-amino-5-oxo-5,6,7,8-tetrahydro-4H-chromenes.

    Science.gov (United States)

    Kumar, Dalip; Reddy, V Buchi; Sharad, Shashwat; Dube, Urvashi; Kapur, Suman

    2009-09-01

    A facile one-pot expeditious synthesis of 2-amino-4H-pyrans and 2-amino-5-oxo-5,6,7,8-tetrahydro-4H-chromenes has been described under solvent-free conditions using magnesium oxide as a catalyst in very good yields. The reaction catalyst, magnesium oxide was reused and recycled without any loss of activity and product yield. All the synthesized compounds were screened for in vitro antibacterial activity, and compounds 3a, 3b, 3f, 4b, 4c, 4d, 4e and 4g showed complete inhibition of bacterial growth at 128 microg/mL or less and the rest of the compounds exhibited incomplete inhibition.

  18. Synthesis, characterization and catalytic application of silica supported tin oxide nanoparticles for synthesis of 2,4,5-tri and 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2017-02-01

    Full Text Available Highly efficient and eco-friendly, one pot synthesis of 1,2,4,5-tetra substituted imidazoles and 2,4,5-trisubstituted imidazoles was reported under solvent free conditions using nanocrystalline silica supported tin oxide (SiO2:SnO2 as a catalyst with excellent yield. The present methodology offers several advantages such as mild reaction conditions, short reaction time, good yield, high purity of product, recyclable catalyst without a noticeable decrease in catalytic activity and can be used for large scale synthesis. The synthesized SiO2:SnO2 nanocrystalline catalyst was characterized by XRD, BET surface area and TEM techniques.

  19. Facile and rapid synthesis of divers xanthene derivatives using lanthanum(III chloride/chloroacetic acid as an efficient and reusable catalytic system under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Pouramiri Behjat

    2017-01-01

    Full Text Available LaCl3/ClCH2COOH was used as an efficient, and recyclable catalytic system for synthesis of 11H-benzo[a]xanthene-11-one, hexahydro-1H-xanthene- 1,8(2H-dione and 11-aryl-10H-diindeno[1,2-b:2′,1′-e]pyran-10,12(11H-dione derivatives via a one-pot three-component reaction of aldehydes, 2-naphthol, and cyclic 1,3-dicarbonyl compounds. The reactions proceeded rapidly at 70°C under solvent-free conditions and the desired products were obtained in good to excellent yields.

  20. One-Pot Isomerization–Cross Metathesis–Reduction (ICMR) Synthesis of Lipophilic Tetrapeptides

    Science.gov (United States)

    2015-01-01

    An efficient, versatile and rapid method toward homologue series of lipophilic tetrapeptide derivatives (herein, the opioid peptides H-TIPP-OH and H-DIPP-OH) is reported. High atom economy and a minimal number of synthetic steps resulted from a one-pot tandem isomerization-cross metathesis-reduction sequence (ICMR), applicable both in solution and solid phase methodology. The broadly applicable synthesis proceeds with short reaction times and simple work-up, as illustrated in this work for alkylated opioid tetrapeptides. PMID:24906051

  1. One-Pot Synthesis and Transmembrane Chloride Transport Properties of C3-Symmetric Benzoxazine Urea.

    Science.gov (United States)

    Roy, Arundhati; Saha, Debasis; Mukherjee, Arnab; Talukdar, Pinaki

    2016-11-18

    One-pot synthesis of a C 3 -symmetric benzoxazine-based tris-urea compound is discussed. 1 H NMR titrations indicate a stronger Cl - binding compared that of Br - and I - by the receptor. Effective Cl - transport across liposomal membranes via a Cl - /X - antiport mechanism is confirmed. Theoretical calculation suggests that a few water molecules with N-H, C═O, and the aromatic ring of the receptor create a H-bonded polar cavity where a Cl - is recognized by O-H···Cl - interactions from five bridged water molecules.

  2. One-Pot Exfoliation of Graphite and Synthesis of Nanographene/Dimesitylporphyrin Hybrids

    Directory of Open Access Journals (Sweden)

    M. Mar Bernal

    2015-05-01

    Full Text Available A simple one-pot process to exfoliate graphite and synthesize nanographene-dimesitylporphyrin hybrids has been developed. Despite the bulky mesityl groups, which are expected to hinder the efficient π–π stacking between the porphyrin core and graphene, the liquid-phase exfoliation of graphite is significantly favored by the presence of the porphyrins. Metallation of the porphyrin further enhances this effect. The resulting graphene/porphyrin hybrids were characterized by spectroscopy (UV-visible, fluorescence, and Raman and microscopy (STEM, scanning transmission electron microscopy.

  3. Electrolytic copper as cheap and effective catalyst for one-pot triazole synthesis.

    Science.gov (United States)

    Mularski, Jacek; Czaplińska, Barbara; Cieślik, Wioleta; Bebłot, Jakub; Bartczak, Piotr; Sitko, Rafał; Polański, Jarosław; Musiol, Robert

    2018-03-14

    Electrolytic copper is a well-known form of pure, oxygen free copper that is used for industrial applications. In this work, the catalytic potential of this relatively cheap material was studied. The addition of less than 0.015 mol equivalent of copper powder effectively catalysed the one-pot synthesis of triazoles from a diverse range of organic halides and alkynes. Quantitative conversions in aqueous solvents can be achieved within minutes. The heterogenous nature of the catalyst afforded a low level of copper contamination in the products, thus meeting the rigorous criteria of the pharmaceutical industry.

  4. One-pot synthesis of 2-aryl-1,2-fused pyrimidones

    Indian Academy of Sciences (India)

    Vol. 129, No. 3, March 2017, pp. 329–333. c Indian Academy of Sciences. DOI 10.1007/s12039-017-1244-z. REGULAR ARTICLE. One-pot synthesis of 2-aryl-1 .... 165.9/(407±55;B.p./. ◦. C)19. 15. 1c. 2d (7-azaindole). 3cd. 42. 178.0. 16. 1d. 2b (C6H5). 3db. 45. 134.2/(396±45;B.p./. ◦. C)20. 17. 1d. 2e (4-F-C6H4). 3de. 47.

  5. One-Pot Multi-Enzymatic Synthesis of the Four Stereoisomers of 4-Methylheptan-3-ol

    Directory of Open Access Journals (Sweden)

    Elisabetta Brenna

    2017-09-01

    Full Text Available The use of pheromones in the integrated pest management of insects is currently considered a sustainable and environmentally benign alternative to hazardous insecticides. 4-Methylheptan-3-ol is an interesting example of an insect pheromone, because its stereoisomers are active towards different species. All four possible stereoisomers of this compound were prepared from 4-methylhept-4-en-3-one by a one-pot procedure in which the two stereogenic centres were created during two sequential reductions catalysed by an ene-reductase (ER and an alcohol dehydrogenase (ADH, respectively.

  6. One-pot synthesis of aryl sulfones from organometallic reagents and iodonium salts.

    Science.gov (United States)

    Margraf, Natalie; Manolikakes, Georg

    2015-03-06

    A transition-metal-free arylation of lithium, magnesium, and zinc sulfinates with diaryliodonium salts is described. The sulfinic acid salts were prepared from the reaction of the corresponding organometallic reagents and sulfur dioxide. Combination of the three single steps (preparation of the organometallic compound, sulfinate formation, and arylation) leads to a one-pot sequence for the synthesis of aryl sulfones from simple starting materials. The chemoselectivity of unsymmetrical diaryliodonium salts has been investigated. Potential and limitations of this method will be discussed.

  7. Seed mediated one-pot growth of versatile heterogeneous upconversion nanocrystals for multimodal bioimaging

    Science.gov (United States)

    Wen, Shihui; Li, Du; Liu, Deming; Xu, Xiaoxue; Du, Yi; Mitchell, David R. G.; Shi, Bingyang; Shi, Xiangyang; Jin, Dayong

    2016-12-01

    The rapid development of a variety of molecular contrast agents makes the multimodality bioimaging highly attractive towards higher resolution, more sensitive, informative diagnosis. The key lies in the development of facile material synthesis that allows the integration of multiple contrast agents, ideally in a way that each of the components should be logically assembled to maximize their performances. Here, we report the one-pot programmable growth of multifunctional heterogeneous nanocrystal with tunable size, shape, composition, and properties. We demonstrated a facile one-pot hot-injection method to enable the highly selectively controlled growth of different sodium lanthanide fluoride nanomaterials in either longitudinal or transversal directions with atomic scale precision. This technique allows the upconversion luminescence signal, MRI signal and x-ray signal logically integrated and optimized within one single versatile nanoplatform for multimode bioimaging. These findings suggest that the facile strategy developed here have the promising to get the desired heterogeneous nanocrystals as an all-in-one contrast agent for integrated and self-correlative multimodal bioimaging.

  8. Direct synthesis of water dispersible superparamagnetic TGA capped FePt nanoparticles: One pot, one shot

    Energy Technology Data Exchange (ETDEWEB)

    Jha, Deepak K. [Department of Physics, Tezpur University (Central University), Tezpur 784028 (India); Varadarajan, Komanduri S.; Patel, Anant B. [Center for Cellular and Molecular Biology, Uppal Road, Hyderabad 500007 (India); Deb, Pritam, E-mail: pdeb@tezu.ernet.in [Department of Physics, Tezpur University (Central University), Tezpur 784028 (India)

    2015-04-15

    Thioglycolic acid (TGA) capped hydrophilic fcc-FePt magnetic nanoparticles (MNPs) were directly synthesized by a facile one pot polyol method. Thioglycolic acid (TGA) was used to functionalize the nanoparticles by incorporating thiol group onto the surface. It helped in the preparation of highly stable dispersions of nanoparticles with spherical morphology. A possible formation mechanism for these FePt MNPs, depending on the role of TGA, was proposed. The as-prepared FePt MNPs possessed a face centered cubic structure with an average size of 6 ± 1 nm and superparamagnetic property at room temperature. MRI study showed that these MNPs exhibited a transverse relaxivity of ∼600 mg{sup −1} ml s{sup −1}, superior to that of reported iron oxide nanoparticles. - Highlights: • One pot synthesis of TGA capped hydrophilic FePt superparamagnetic nanoparticles. • Role of TGA molecules in the formation of FePt nanoparticles. • EDX reveals the equiatomic ratio of Fe and Pt atoms in FePt nanoparticles. • The HR-TEM exhibits spherical nanoparticles with a narrow size distribution. • High transverse relaxivity suggesting as potential MRI contrast agent.

  9. Synthesis of hybrid Au–ZnO nanoparticles using a one pot polyol process

    Energy Technology Data Exchange (ETDEWEB)

    Mezni, Amine [Unité de recherche “Synthèse et Structure de Nanomatériaux” UR11ES30, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Jarzouna (Tunisia); Centre d' Elaboration de Matériaux et d' Etudes Structurales, CNRS, UPR 8011, Université de Toulouse, 29 Rue Jeanne Marvig, 31055 Toulouse (France); Mlayah, Adnen; Serin, Virginie [Centre d' Elaboration de Matériaux et d' Etudes Structurales, CNRS, UPR 8011, Université de Toulouse, 29 Rue Jeanne Marvig, 31055 Toulouse (France); Smiri, Leila Samia, E-mail: lsmiri@gmail.com [Unité de recherche “Synthèse et Structure de Nanomatériaux” UR11ES30, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Jarzouna (Tunisia)

    2014-10-15

    In this work, we report on the synthesis of hybrid Au–ZnO nanoparticles using a one-pot chemical method that makes use of 1,3-propanediol as a solvent, a reducing agent and a stabilizing layer. The produced nanoparticles consisted of Au cores decorated with ZnO nanoparticles. The structure and morphology of the nanoparticles were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDX) and Raman spectroscopy. Optical extinction measurements, combined with numerical simulations, showed that the Au–ZnO nanoparticles exhibit a localized surface plasmon resonance (SPR) clearly red-shifted with respect to that of bare Au nanoparticles (AuNPs). This work contributes to the emergence of multi-functional nanomaterials with possible applications in surface plasmon resonance based biosensors, energy-conversion devices, and in water-splitting hydrogen production. - Highlights: • Hybrid Au–ZnO nanoparticles were synthesized by a novel one-pot synthesis method that makes use of 1,3-propanediol. • The polyol solvent 1,3-propanediol plays the roles of the reducing agent and the stabilizer layer. • The Au–ZnO nanoparticles exhibit a strong localized surface plasmon resonance.

  10. Novel one-pot route to monodisperse thermosensitive hollow microcapsules in a microfluidic system.

    Science.gov (United States)

    Choi, Chang-Hyung; Jung, Jae-Hoon; Kim, Dong-Wan; Chung, Young-Min; Lee, Chang-Soo

    2008-09-01

    We present a simple one-pot synthetic approach for the preparation of monodisperse thermo-sensitive poly(N-isopropylacrylamide) (PNIPAM) microcapsules in a microfluidic system. Based on the mechanism of shear force-driven break-off, aqueous droplets of monomer solution are continuously generated in an immiscible continuous phase containing photoinitiators. Under UV irradiation, activated initiators are diffused into the interface between the continuous phase and the aqueous droplets, which trigger polymerization of NIPAM monomers. The PNIPAM microcapsules produced are hollow microcapsules with a thin shell membrane, high monodispersity, and fast response to environmental temperature. In addition, the size of microcapsules produced can be manipulated by the flow rate of the continuous phase or aqueous phase and different concentrations of surfactant to control interfacial tension between continuous phase and aqueous phase. Furthermore, the versatility of this approach enables the preparation of monodisperse microcapsules having the capability to encapsulate various materials such as proteins and nanoparticles under mild conditions. The in situ microfluidic synthetic method provides a novel approach for the preparation of monodisperse hollow microcapsules via a one-pot route.

  11. One-pot native chemical ligation of peptide hydrazides enables total synthesis of modified histones.

    Science.gov (United States)

    Li, Jiabin; Li, Yuanyuan; He, Qiaoqiao; Li, Yiming; Li, Haitao; Liu, Lei

    2014-08-07

    One of the rising demands in the field of protein chemical synthesis is the development of facile strategies that yield the protein in workable quantities and homogeneity, with fewer handling steps. Although the native chemical ligation of peptide hydrazides has recently been shown to be useful for the chemical synthesis of proteins carrying acid-sensitive modification groups, previous hydrazide-based protein synthesis studies have used sequential ligation strategies. Here, we report a practical method for a "one-pot" native chemical ligation of peptide hydrazides that would circumvent the need for the isolation of the intermediate products. This method employed a fast and selective arylboronate oxidation reaction mediated by H2O2, which draws attention to the potential applications of the thus far under-exploited boron-based functionalities in protein chemical synthesis. To demonstrate the practicality and efficiency of the new one-pot method, we report its application to a scalable total synthesis of modified histones (with five analogues of H3 and H4 as examples) on a multi-milligram scale, with good homogeneity.

  12. One-pot synthesis of Ag-SiO2-Ag sandwich nanostructures

    International Nuclear Information System (INIS)

    Li Chaorong; Mei Jie; Li Shuwen; Lu Nianpeng; Wang Lina; Chen Benyong; Dong Wenjun

    2010-01-01

    Ag-SiO 2 -Ag sandwich nanostructures were prepared by a facile one-pot synthesis method. The Ag core, SiO 2 shell and Ag nanoparticle shell were all synthesized with polyvinylpyrrolidone, catalysed by ammonia, in the one-pot reaction. The polyvinylpyrrolidone, acting as a smart reducing agent, reduced the Ag + to Ag cores and Ag shells separately. Furthermore, the polyvinylpyrrolidone served as a protective agent to prevent the silver cores from aggregating. The SiO 2 shell and outer layer Ag nanoparticles were obtained when tetraethyl orthosilicate and ammonia were added to the silver core solution. Ammonia, acting as the catalyst, accelerated the hydrolysis of the tetraethyl orthosilicate to SiO 2 , which coated the silver cores. Furthermore, Ag(NH 3 ) 2 + ions were formed when aqueous ammonia was added to the solution, which increased the reduction capability. Then the polyvinylpyrrolidone reduced the Ag(NH 3 ) 2 + ions to small Ag nanoparticles on the surface of the Ag-SiO 2 and formed Ag-SiO 2 -Ag sandwich structures with a standard deviation of less than 4%. This structure effectively prevented the Ag nanoparticles on the silica surface from aggregating. Furthermore, the Ag-SiO 2 -Ag sandwich structures showed good catalysis properties due to the large surface area/volume value and activity of surface atoms of Ag particles.

  13. Assembly of a biocompatible triazole-linked gene by one-pot click-DNA ligation

    Science.gov (United States)

    Kukwikila, Mikiembo; Gale, Nittaya; El-Sagheer, Afaf H.; Brown, Tom; Tavassoli, Ali

    2017-11-01

    The chemical synthesis of oligonucleotides and their enzyme-mediated assembly into genes and genomes has significantly advanced multiple scientific disciplines. However, these approaches are not without their shortcomings; enzymatic amplification and ligation of oligonucleotides into genes and genomes makes automation challenging, and site-specific incorporation of epigenetic information and/or modified bases into large constructs is not feasible. Here we present a fully chemical one-pot method for the assembly of oligonucleotides into a gene by click-DNA ligation. We synthesize the 335 base-pair gene that encodes the green fluorescent protein iLOV from ten functionalized oligonucleotides that contain 5ʹ-azide and 3ʹ-alkyne units. The resulting click-linked iLOV gene contains eight triazoles at the sites of chemical ligation, and yet is fully biocompatible; it is replicated by DNA polymerases in vitro and encodes a functional iLOV protein in Escherichia coli. We demonstrate the power and potential of our one-pot gene-assembly method by preparing an epigenetically modified variant of the iLOV gene.

  14. Lanthanide nitrates as Lewis acids in the one-pot synthesis of 1,2,4-oxadiazole derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Vale, Juliana A.; Faustino, Wagner M., E-mail: julianadqf@yahoo.com.br [Departamento de Quimica, Universidade Federal da Paraiba, Joao Pessoa, PB (Brazil); Zampieri, Davila de S.; Moran, Paulo J.S.; Rodrigues, Jose A.R. [Instituto de Quimica, Universidade Estadual de Campinas, SP (Brazil); Sa, Gilberto F. de [Departamento de Quimica Fundamental, CCEN, Universidade Federal de Pernambuco, Recife, PE (Brazil)

    2012-08-15

    In this work we report the use of lanthanide nitrates [Ln(NO{sub 3}){sub 3}] acting as catalyst in direct one pot synthesis of 3-benzoyl- and 3-acetyl-1,2,4-oxadiazoles derivatives from ketones, nitriles and nitric acid. This is the first example of one-pot synthesis of benzoyl- and acetyl 1,2,4-oxadiazoles derivatives preparation using acetophenones derivates with electron-donator groups. (author)

  15. Solvent-free covalent functionalization of nanodiamond with amines

    International Nuclear Information System (INIS)

    Basiuk, Elena V.; Santamaría-Bonfil, Adriana; Meza-Laguna, Victor; Gromovoy, Taras Yu.; Alvares-Zauco, Edgar; Contreras-Torres, Flavio F.; Rizo, Juan; Zavala, Guadalupe; Basiuk, Vladimir A.

    2013-01-01

    Covalent functionalization of pristine nanodiamond (ND) with 1,12-diaminododecane (DAD), 1,5-diaminonaphthalene (DAN), poly(ethylene glycol) diamine (PEGDA), and polyethylenimine (PEI) was carried out by employing solvent-free methodology, which is based on thermal instead of chemical activation of carboxylic groups at ND surface. A simple solubility/dispersibility test in water and isopropanol showed an increased lipophilicity of the functionalized samples. The conversion of intrinsic carboxylic groups into the corresponding amide derivatives was characterized by means of Fourier-transform infrared spectroscopy. Thermogravimetric analysis found the highest organic content of about 18% for ND-PEI, followed by ND-DAD, for which the contribution of covalently bonded diamine was estimated to be of ca. 10%. In temperature programmed desorption measurements with mass spectrometric detection, the presence of organic functionalizing groups changed both mass spectra and thermodesorption curves of ND. The changes in morphology of primary and secondary ND aggregates were characterized by scanning and transmission electron microscopy, as well as by atomic force microscopy. The current–voltage measurements under atmospheric pressure found an increased conductivity for ND-DAN, as compared to that of pristine ND, whereas for ND-DAD, ND-PEGDA and ND-PEI a dramatic decrease in conductivity due to functionalization was observed.

  16. Solvent-free covalent functionalization of nanodiamond with amines

    Energy Technology Data Exchange (ETDEWEB)

    Basiuk, Elena V., E-mail: elenagd@unam.mx [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Santamaría-Bonfil, Adriana; Meza-Laguna, Victor [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Gromovoy, Taras Yu. [Institute of Surface Chemistry, National Academy of Sciences of the Ukraine, Gen. Naumova 17, 03164 Kiev (Ukraine); Alvares-Zauco, Edgar [Facultad de Ciencias, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Contreras-Torres, Flavio F.; Rizo, Juan [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Zavala, Guadalupe [Instituto de Biotecnología, Universidad Nacional Autónoma de México, Av. Universidad 2001, Col. Chamilpa, 62210, Cuernavaca, Morelos (Mexico); Basiuk, Vladimir A. [Instituto de Ciencias Nucleares, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México, D.F. (Mexico)

    2013-06-15

    Covalent functionalization of pristine nanodiamond (ND) with 1,12-diaminododecane (DAD), 1,5-diaminonaphthalene (DAN), poly(ethylene glycol) diamine (PEGDA), and polyethylenimine (PEI) was carried out by employing solvent-free methodology, which is based on thermal instead of chemical activation of carboxylic groups at ND surface. A simple solubility/dispersibility test in water and isopropanol showed an increased lipophilicity of the functionalized samples. The conversion of intrinsic carboxylic groups into the corresponding amide derivatives was characterized by means of Fourier-transform infrared spectroscopy. Thermogravimetric analysis found the highest organic content of about 18% for ND-PEI, followed by ND-DAD, for which the contribution of covalently bonded diamine was estimated to be of ca. 10%. In temperature programmed desorption measurements with mass spectrometric detection, the presence of organic functionalizing groups changed both mass spectra and thermodesorption curves of ND. The changes in morphology of primary and secondary ND aggregates were characterized by scanning and transmission electron microscopy, as well as by atomic force microscopy. The current–voltage measurements under atmospheric pressure found an increased conductivity for ND-DAN, as compared to that of pristine ND, whereas for ND-DAD, ND-PEGDA and ND-PEI a dramatic decrease in conductivity due to functionalization was observed.

  17. Silica-supported boric acid with ionic liquid: a novel recyclable catalytic system for one-pot three-component Mannich reaction.

    Science.gov (United States)

    Kumar, Vishal; Sharma, Upendra; Verma, Praveen Kumar; Kumar, Neeraj; Singh, Bikram

    2011-01-01

    A rapid and efficient silica-supported boric acid/ionic liquid ([bmim][PF₆]), catalyzed, one-pot three-component Mannich reaction has been carried out to synthesize β-amino carbonyl compounds at room temperature. The reaction afforded desired products in excellent yields with moderate to good diastereoselectivity. The method provides a novel modification of three-component Mannich reaction in terms of mild reaction conditions, clean reaction profiles, low amount of catalyst, recyclability of catalyst and a simple workup procedure. The present report first time describes the preparation of H₃BO₃-SiO₃ catalyst and its use with [bmim][PF₆], to synthesize Mannich products. The catalyst can be reused at least seven times.

  18. Direct biocatalytic one-pot-transformation of cyclohexanol with molecular oxygen into ɛ-caprolactone.

    Science.gov (United States)

    Staudt, Svenja; Bornscheuer, Uwe T; Menyes, Ulf; Hummel, Werner; Gröger, Harald

    2013-09-10

    The development of a biocatalytic process concept for ɛ-caprolactone, which directly converts cyclohexanol as an easily available industrial raw material into the desired ɛ-caprolactone in a one-pot fashion while only requiring air as sole reagent, is reported. The desired product ɛ-caprolactone was obtained with 94-97% conversion when operating at a substrate concentration in the range of 20-60 mM. At higher substrate concentrations, however, a significant drop of conversion was found. Subsequent detailed studies on the impact of the starting material, intermediate and product components revealed a significant inhibition and partial deactivation of the BVMO by the product ɛ-caprolactone (in particular at higher concentrations) as well as an inhibition of the BVMO by cyclohexanol and cyclohexanone. Copyright © 2013 Elsevier Inc. All rights reserved.

  19. A one-pot chemoselective synthesis of secondary amines by using a biomimetic electrocatalytic system

    International Nuclear Information System (INIS)

    Largeron, Martine

    2009-01-01

    A one-pot electrochemically induced oxidation-imine formation-reduction route to secondary amines is described in detail. The key step of the process consists of the o-iminoquinone-mediated chemoselective catalytic oxidation of a primary aliphatic amine substrate, in the presence of a second amine used as the alkylating agent. Through the examination of the scope of the reaction by systematically varying both amine substrate and amine alkylating agent, it can be shown that this reaction sequence, leaving ammonia as the sole by-product, allows the rapid synthesis of various secondary amines in moderate to good yields. This process, that highlights the pre-eminent green advantages of electrochemical synthesis, especially the utilization of electricity as energy instead of chemical reagents, high atom economy as well as ambient temperature and pressure, could be a mild alternative to already reported synthetic methods.

  20. One-pot synthesis of graphene oxide sheets and graphene oxide quantum dots from graphite nanofibers

    Energy Technology Data Exchange (ETDEWEB)

    Abdul Rashid, Suraya, E-mail: suraya-ar@upm.edu.my; Mohd Zobir, Syazwan Afif [Universiti Putra Malaysia, Materials Processing and Technology Laboratory, Nanomaterials and Nanotechnology Group, Institute of Advanced Technology (Malaysia); Krishnan, Shutesh; Hassan, Mohd Murshid [Graphene Nanochem Sdn. Bhd., Level 9, WORK@Clearwater (Malaysia); Lim, Hong Ngee [Universiti Putra Malaysia, UPM, Department of Chemistry, Faculty of Science (Malaysia)

    2015-05-15

    A one-pot synthesis of graphene oxide (GO) sheets and GO quantum dots using graphite nanofibers (GNF) as starting material is reported. Two types of GNF starting materials, namely herringbone and platelet structures, were used. HRTEM revealed that platelet GNF produces quantum dots typically less than 10 nm in size while herringbone GNF produces relatively larger GO sheets. SAED patterns indicate that the produced GO sheets have a hexagonal crystal structure. UV–Vis, PL, XPS, and Raman show salient differences between the produced GO nanostructures which correlate well with the morphological analysis. Unlike the GO sheets, the GO quantum dots are photoluminescent. The difference in PL properties was attributed to the higher oxygen content in GO quantum dots which were shown by XPS. The results offer a new insight to the importance of starting material in the synthesis of graphene nanostructures.

  1. Facile One-Pot Polyol Method for the Synthesis of Uniform Size Silver Nanowires.

    Science.gov (United States)

    Kaili, Zhang; Yongguo, Du; Shimin, Chen

    2016-01-01

    This study reports the development of a facile and efficient one-pot polyol method for the synthesis of silver nanowires. The seed and growth of silver nanowires under different reaction conditions were characterized and measured. The pertinent variables such as temperature, time, concentration and capping agent were investigated. Moreover, the effect of seeding at two different stages-initial stage and secondary stage-was studied and discussed on the size control of silver nanowires. In particular, silver nanowires with diameter less than 40 nm and length over 25 µm in a narrow distribution, was obtained through a novel method in which reaction flask was placed in a low-temperature bath after seeding for some time in the high-temperature bath. This approach may be useful for the fabrication of uniform, large aspect ratio silver nanowires for optoelectronic applications.

  2. One-pot environmentally friendly approach toward highly catalytically active bimetal-nanoparticle-graphene hybrids.

    Science.gov (United States)

    Liu, Chang-Hai; Chen, Xiao-Qi; Hu, Yong-Feng; Sham, Tsun-Kong; Sun, Qi-Jun; Chang, Jian-Bing; Gao, Xu; Sun, Xu-Hui; Wang, Sui-Dong

    2013-06-12

    A one-pot universal approach with simple metal sputtering onto room temperature ionic liquids has been developed to prepare bimetal-nanoparticle (NP)-graphene hybrids, and the process is environmentally friendly and completely free of additives and byproducts. The graphene-supported bimetallic NPs have an Ag-based core and an Au/Pd-rich shell, demonstrated by the scanning transmission electron microscopy. The X-ray absorption near-edge spectroscopy using synchrotron radiation reveals the occurrence of charge redistribution at both the Ag@Au and Ag@Pd core-shell interfaces. The as-prepared Ag@Au and Ag@Pd bimetal-NP-graphene hybrids are highly catalytically active for reduction of 4-nitrophenol, whose catalytic activity is superior to the corresponding monometallic hybrids. The catalytic superiority is ascribed to the electronic structure modification and morphological irregularity of the graphene-supported bimetallic NPs.

  3. One-pot synthesis and bioapplication of amine-functionalized magnetite nanoparticles and hollow nanospheres.

    Science.gov (United States)

    Wang, Leyu; Bao, Jie; Wang, Lun; Zhang, Fang; Li, Yadong

    2006-08-16

    To demonstrate their applications in biological and medical fields such as in immunoassays, magnetic separation of cells or proteins, drug or gene delivery, and magnetic resonance imaging, the template-free syntheses of water-soluble and surface functionalized magnetic nanomaterials have become essential and are challenging. Herein, we developed a facile one-pot template-free method for the preparation of amine-functionalized magnetite nanoparticles and hollow nanospheres by using FeCl(3)6 H(2)O as single iron source. These magnetic nanomaterials were characterized by TEM, SEM, XRD, and FTIR technologies. Their magnetic properties were also studied by using a superconducting quantum interference device (SQUID) magnetometer at room temperature. Then the amine-functionalized magnetite nanoparticles were applied to immunoassays and magnetic resonance imaging in live mice.

  4. Reducing size-dispersion in one-pot aqueous synthesis of maghemite nanoparticles.

    Science.gov (United States)

    Drummond, A L; Feitoza, N C; Duarte, G C; Sales, M J A; Silva, L P; Chaker, J A; Bakuzis, A F; Sousa, M H

    2012-10-01

    Nanosized maghemite-like particles with reduced size-distribution were obtained using a one-pot synthesis route in aqueous medium. Forced hydrolysis of iron ions in ammoniac solution led to the formation of magnetite nanoparticles that were oxidized to maghemite in a hydrothermal digestion step that reduced the polydispersity of nanograins. The prepared nanoparticles were characterized by chemical analysis, X-ray diffractometry, magnetization, Raman spectroscopy and transmission electron microscopy measurements. Data showed that 14 nm-sized particles with polydispersity of about 0.14 were produced and, differently from other procedures, neither additional steps nor toxic reagents were needed to reduce size-dispersion or to oxidize magnetite to maghemite. These facts per se turn such nanodevice into a good potential choice for biomedical applications.

  5. Polymeric Nanocapsule from Silica Nanoparticle@Cross-linked Polymer Nanoparticles via One-Pot Approach

    Directory of Open Access Journals (Sweden)

    Shen Ruoping

    2009-01-01

    Full Text Available Abstract A facile strategy was developed here to prepare cross-linked polymeric nanocapsules (CP nanocapsules with silica nanoparticles as templates. The silica nanoparticle@cross-linked polymer nanoparticles were prepared by the encapsulation of the silica nanoparticles by the one-pot approach via surface-initiated atom transfer radical polymerization of hydroxyethyl acrylate in the presence ofN,N′-methylenebisacrylamide as a cross-linker from the initiator-modified silica nanoparticles. After the silica nanoparticle templates were etched with hydrofluoric acid, the CP nanocapsules with particle size of about 100 nm were obtained. The strategy developed was confirmed with Fourier transform infrared, thermogravimetric analysis and transmission electron microscopy.

  6. One-pot organometallic synthesis of alumina-embedded Pd nanoparticles.

    Science.gov (United States)

    Costa, Natália J S; Vono, Lucas L R; Wojcieszak, Robert; Teixiera-Neto, Érico; Philippot, Karine; Rossi, Liane M

    2017-10-24

    Herein we report a one pot organometallic strategy to access alumina-embedded Pd nanoparticles. Unexpectedly, the decomposition of the organometallic complex tris(dibenzylideneacetone)dipalladium(0), Pd 2 (dba) 3 , by dihydrogen in the presence of aluminum isopropoxide, Al(iPrO) 3 , and without extra stabilizers, was found to be an efficient method to generate a Pd colloidal solution. Careful characterization studies revealed that the so-obtained Pd nanoparticles were stabilized by an aluminum isopropoxide tetramer and 1,5-diphenyl-pentan-3-one, which was produced after reduction of the dba ligand from the organometallic precursor. Moreover, calcination of the obtained nanomaterial in air at 773 K for 2 h resulted in a nanocomposite material containing Pd nanoparticles embedded in Al 2 O 3 . This stabilization strategy opens new possibilities for the preparation of transition metal nanoparticles embedded in oxides.

  7. B(C6F5)3 catalyzed one-pot three-component Biginelli reaction: An ...

    Indian Academy of Sciences (India)

    applications in drug industries.4g,h The expansion of natural products chemistry with structural diversifi- cation of dihydropyrimidinone motif also found syn- thetic attention from Biginelli reaction. Therefore, there has been continuous interest from organic and medicinal chemists towards the development of milder and more ...

  8. B(C6F5)3 catalyzed one-pot three-component Biginelli reaction: An ...

    Indian Academy of Sciences (India)

    sulfonated β-cyclodextrine,7f hexaaquaaluminium(III) tetrafluoro- borate,7g zeolite7h and polyoxometalate7i have been developed. Many other synthetic approaches including combinatorial approach,8a microwave,8b sonication,8c ionic liquids8d and organocatalysts8e have been actively pursued for the preparation of ...

  9. Continuous metal scavenging and coupling to one-pot copper-catalyzed azide-alkyne cycloaddition click reaction in flow

    NARCIS (Netherlands)

    Vural - Gursel, Dr. Iris; Aldiansyah, Ferry; Wang, Qi; Noël, Timothy; Hessel, Volker

    2015-01-01

    Increasing usage of catalytic chemistry calls for efficient removal of metal traces. This paper describes the development and optimization of a scavenger-based extraction in flow to remove metal catalysts. It enables liquid-liquid extraction with slug flow and phase separation with a porous

  10. Solvent-free synthesis of azomethines, spectral correlations and antimicrobial activities of some E-benzylidene-4-chlorobenzenamines

    Directory of Open Access Journals (Sweden)

    R. Suresh

    2015-07-01

    Full Text Available Some azomethines including substituted benzylidene-4-chlorobenzenamines (E-imines have been synthesized by fly-ash: PTS catalyzed microwave assisted condensation of 4-chloroaniline and substituted benzaldehydes under solvent-free conditions. The yield of the imines has been found to be more than 85%. The purity of all imines has been checked using their physical constants and UV, IR and NMR spectral data. These spectral data have been correlated with Hammett substituent constants and F and R parameters using single and multi-linear regression analysis. From the results of statistical analysis, the effect of substituents on the above spectral data has been studied. The antimicrobial activities of all imines have been studied using standard methods.

  11. One-pot synthesis of magnetic, macro/mesoporous bioactive glasses for bone tissue engineering

    Directory of Open Access Journals (Sweden)

    Dan Wang, Huiming Lin, Jingjie Jiang, Xiao Han, Wei Guo, Xiaodan Wu, Yingxue Jin and Fengyu Qu

    2013-01-01

    Full Text Available Magnetic and macro/mesoporous bioactive glasses were synthesized by a one-pot method via a handy salt leaching technique. It was identified to be an effective and simple synthetic strategy. The non-ionic triblock copolymer, poly(ethylene glycol-block-poly(propylene glycol-block-poly(ethylene glycol (P123, was used as the structure directing agent for mesoporous structure but also as the reductant to reduce the iron source into magnetic iron oxide. The prepared materials exhibited excellent super-paramagnetic property with interconnected macroporous (200–300 μm and mesoporous (3.4 nm structure. Furthermore, their outstanding drug storage/release properties and rapid (5 induction of hydroxyapatite growth ability were investigated after immersing in simulated body fluid solution at 37 °C. Notably, the biocompatibility assessment confirmed that the materials obtained presented good biocompatibility and enhanced adherence of HeLa cells. Herein, the novel materials are expected to have potential application for bone tissue engineering.

  12. One-pot fabrication and antimicrobial properties of novel PET nonwoven fabrics.

    Science.gov (United States)

    Lin, Song; Wang, Zheng; Qi, Jian-cheng; Wu, Jin-hui; Tian, Tao; Hou, Li-li; Hao, Li-mei; Yang, Jing-quan

    2011-08-01

    Recently, with the ever-growing demand for healthy living, more and more research is focused on materials capable of killing harmful microorganisms around the world. It is believed that designing such protective materials for hygienic and biomedical applications can benefit people in professional areas and daily life. Thus, in this paper, one novel kind of antibacterial poly(ethylene terephthalate) (PET) nonwoven fabrics was conveniently one-pot prepared, with the combined immobilization of two biological antimicrobial agents, i.e. ε-polylysine and natamycin, by using the soft methacrylate nonwoven fabrics adhesives. Then, the antimicrobial activities of the functional fabrics were investigated by using the standard shaking-flask method, showing excellent antibacterial efficiency (AE) against both Escherichia coli (8099) and Staphylococcus aureus (ATCC 6538) (AE > 99.99%) compared with untreated PET nonwoven fabrics. The anti-bioaerosol tests also showed similar trends. Meantime, scanning electron microscopy analysis indicated that the bacteria on the antibacterial PET appeared to be partly bacteriolyzed and showed much less viability than those on the pristine ones. Moreover, the long residual biocidal action of such modified PET fabrics was also evaluated, and the antibacterial activity of antibacterial fibers was unaffected by the 3 month artificially accelerated aging. © 2011 IOP Publishing Ltd

  13. One-pot size-controlled growth of graphene-encapsulated germanium nanocrystals

    Science.gov (United States)

    Lee, Jae-Hyun; Lee, Eun-Kyung; Kang, Seog-Gyun; Jung, Su-Ho; Son, Seok-Kyun; Nam, Woo Hyun; Kim, Tae-Hoon; Choi, Byong Lyong; Whang, Dongmok

    2018-05-01

    To realize graphene-encapsulated semiconductor nanocrystals (NCs), an additional graphene coating process, which causes shape destruction and chemical contamination, has so far been inevitable. We report herein one-pot growth of uniform graphene-germanium core-shell nanocrystals (Ge@G NCs) in gram scale by the addition of methane as a carbon source during the thermal pyrolysis of germane. The methane plays a critical role in the growth of the graphene shell, as well as in the determination of the nucleation density and diameter of the NCs, similar to a surfactant in the liquid-phase growth of monodisperse NCs. By adjusting the gas ratio of precursors, a mixture of germane and methane, we can control the size of the Ge@G NCs in the range of ∼5-180 nm. The Ge@G NCs were characterized by various microscopic and spectroscopic tools, which indicated that the Ge core is single crystalline, and is completely covered by the graphene shell. We further investigated the merits of the graphene shell, which can enhance the electrical conductivity of nanocrystalline materials.

  14. One-pot pseudomorphic crystallization of mesoporous porous silica to hierarchical porous zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Xing, Jun-Ling; Jiang, Shu-Hua; Pang, Jun-Ling; Yuan, En-Hui; Ma, Xiao-Jing [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, College of Chemistry and Molecular Engineering, East China Normal University, No. 3663 Zhongshan North Road, 200062 Shanghai (China); Lam, Koon-Fung [Department of Chemical Engineering, University College London, Torrington Place, London (United Kingdom); Xue, Qing-Song, E-mail: qsxue@chem.ecnu.edu.cn [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, College of Chemistry and Molecular Engineering, East China Normal University, No. 3663 Zhongshan North Road, 200062 Shanghai (China); Zhang, Kun, E-mail: kzhang@chem.ecnu.edu.cn [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, College of Chemistry and Molecular Engineering, East China Normal University, No. 3663 Zhongshan North Road, 200062 Shanghai (China)

    2015-09-15

    Hierarchically porous silica with mesopore and zeolitic micropore was synthesized via pseudomorphic crystallization under high-temperature hydrothermal treatment in the presence of cetyltrimethylammonium tosylate and tetrapropylammonium ions. A combined characterization using small-angle X-ray diffraction (XRD), nitrogen adsorption, high-resolution transmission electron microscopy (TEM), thermogravimetric analysis (TG), and elemental analysis showed that dual templates, CTA{sup +} and TPA{sup +} molecules, can work in a cooperative manner to synthesize mesoporous zeolite in a one-pot system by precisely tuning the reaction conditions, such as reaction time and temperature, and type and amount of heterometal atoms. It is found that the presence of Ti precursor is critical to the successful synthesis of such nanostructure. It not only retards the nucleation and growth of crystalline MFI domains, but also acts as nano-binder or nano-glue to favor the assembly of zeolite nanoblocks. - Graphical abstract: Display Omitted - Highlights: • A facile method to synthesize mesoporous zeolites with hierarchical porosity was presented. • It gives a new insight into keeping the balance between mesoscopic and molecular ordering in hierarchical porous materials. • A new understanding on the solid–solid transformation mechanism for the synthesis of titanosilicate zeolites was proposed.

  15. One pot phytosynthesis of gold nanoparticles using Genipa americana fruit extract and its biological applications

    International Nuclear Information System (INIS)

    Kumar, Brajesh; Smita, Kumari; Cumbal, Luis; Camacho, Javier; Hernández-Gallegos, Elisabeth; Guadalupe Chávez-López, María de; Grijalva, Marcelo; Andrade, Kleber

    2016-01-01

    In this article, rapid one pot synthesis of gold nanoparticles (GNPs) using an eco-friendly extract of Genipa americana L. fruit is described. Electrospray ionization mass spectrometry (ESI-MS) and Fourier transform infrared (FTIR) spectroscopic studies demonstrated that small molecules such as genipin, genipaol, geniposide and ranolazine can act as reducer as well as stabilizers. The monodispersed, spherical GNPs were further characterized by UV–vis spectroscopy at λ max = 535 nm, transmission electron microscopy (TEM), dynamic light scattering (DLS) and X-ray diffraction (XRD) analysis. This synthetic approach offers a greener and alternate route to the preparation of GNPs free from toxic chemical components and stable for 6–7 months under room temperature. The green synthesized GNPs showed weak antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl and no cytotoxicity against A-549 and HeLa human cancer cell lines, from lung and cervix. This study opens a new industrial scope of G. americana fruit in nanoscience and as surface modified GNPs can be developed into a successful drug carrier for future pharmaceutical products. - Highlights: • Gold nanoparticles can be synthesized by Genipa americana fruit extract. • TEM-DLS analysis confirmed that the average particle size is 30.4 ± 14.9 nm. • Nanoparticles showed weak antioxidant and no cytotoxicity activity.

  16. One-pot synthesis and transfer of PMMA/Ag photonic nanocomposites by pulsed laser deposition

    Science.gov (United States)

    Karoutsos, V.; Koutselas, I.; Orfanou, P.; Mpatzaka, Th.; Vasileiadis, M.; Vassilakopoulou, A.; Vainos, N. A.; Perrone, A.

    2015-08-01

    Nanocomposite films comprising metallic nanoparticles in polymer matrices find increasing use in emerging photonic, electronic and microsystem applications owing to their tailored advanced functionalities. The versatile development of such films based on poly-methyl-methacrylate (PMMA) matrix having embedded Ag nanoparticles is addressed here. Two low-cost one-pot chemical methods for the synthesis of bulk target nanocomposite materials are demonstrated. These nanocomposites are subsequently transferred via pulsed laser deposition using 193 nm ArF excimer laser radiation, producing films maintaining the structural and functional properties. Both target- and laser-deposited materials have been thoroughly characterized using microscopic, spectroscopic and thermal analysis methods. Infrared spectra demonstrated the close molecular PMMA chain similarity for both target and film materials, though structural alterations identified by thermal analysis proved the enhanced characteristics of films grown. High-resolution electron microscopy proved the transfer of Ag nanoparticles sized 10-50 nm. Visible absorption peaked in the spectral range of 430-440 nm and attributed to the Ag nanocomposite plasmonic response verifying the transfer of the functional performance from target to film.

  17. Surface morphology of PMMA/boehmite hybrid nanostructures prepared via facile one-pot process

    Science.gov (United States)

    Ghamari, Misagh; Farzi, Gholamali

    2017-08-01

    In this study, we developed the novel aqueous-based PMMA/AlOOH hybrid by a one-pot process starting from their relevant precursors in a controlled manner. Starting chemical reactions directly from precursors and the sequence of adding reactants provide the possibility towards enhancing the homogeneity of the final product. Inorganic and organic segments were made compatible by means of oleic acid as a coupling agent. Boehmite to PMMA weight ratio as the main parameter was varied from 0 to 18% and the morphology, particle size, size distribution, and topography map of hybrids was shown to be composition dependent. Final PMMA/Bo nanohybrids were characterized using FTIR to confirm the chemical interactions between inorganic and organic segments. TEM analysis showed that nanohybrid particles with irregular shapes containing inorganic particles dispersed in the organic matrix are formed with an average diameter which depends on boehmite content. The presence of phase transformation of Bo makes PMMA/Bo hybrids significantly thermally stable. According to AFM topography map analysis and relevant Gaussian fit function, the roughness of nanocomposite, the size of hybrid nanoparticles and deviation from the mean value (size) were increased as Bo increases from 0 to 18.

  18. One pot synthesis of silver nanoparticles using a cyclodextrin containing polymer as reductant and stabilizer

    Directory of Open Access Journals (Sweden)

    Arkadius Maciollek

    2014-03-01

    Full Text Available A facile and one pot synthesis of silver nanoparticles with narrow size distributions using silver nitrate and a copolymer 1 from N-isopropylacrylamide (NIPAM and mono-(1H-triazolylmethyl-2-methylacryl-β-cyclodextrin acting as reductant and stabilizer without using any additional reducing agent is reported. The reduction was carried out in aqueous solution under pH neutral conditions at room temperature. The results of dynamic light scattering analysis and transmission electron microscopy show adjustable particle sizes from 30–100 nm, due to variation of silver nitrate concentration, the polymeric reducing and stabilisation agent concentration or reaction time. The spherical structure of the silver nanoparticles has been confirmed by UV–vis spectroscopy and transmission electron microscopy. The optical properties of the nanoparticles have also been characterized by fluorescence spectroscopy. The formed spherical particles are stable in aqueous medium at room temperature over a period of several weeks. Furthermore the changes in the optical properties of the nanoparticles due to thermo induced volume phase transition behavior of the thermoresponsive cyclodextrin containing polymer 1 have been characterized by UV–vis spectroscopy.

  19. One-pot synthesis of gold/poly(3,4-ethylendioxythiophene) nanocomposite

    International Nuclear Information System (INIS)

    Ventosa, E.; Colina, A.; Heras, A.; Ruiz, V.; Garoz, J.; López-Palacios, J.

    2012-01-01

    In this paper, we report the preparation of highly stable gold nanoparticles/poly(3,4-ethylendioxythiophene) nanocomposites by a one-pot chemical route in aqueous medium without surfactants to increase the solubility of the monomer (3,4-ethylendioxythiophene, EDOT) or to stabilize gold nanoparticles (Au NPs). The generation of the nanocomposite was followed by UV–Visible transmission spectroscopy combined with multivariate curve resolution alternating least squares analysis to deconvolute the individual spectra of the different species generated in the synthesis: oligomers, polymer and gold nanoparticles. The plasmon band observed at 530 nm during the synthesis step indicates the generation of gold nanoparticles. The influence of monomer and metal precursor concentration and their concentration ratios on Au NP size were analyzed. The electrochromic properties of the composite were investigated by UV–Visible absorption spectroelectrochemistry, being mainly related to polymer oxidation and reduction. The main difference observed is the hypsochromic shift of the polymer spectra due to the gold nanoparticles inside the polymer. Multicyclic spectroelectrochemical experiments evidence a high stability and adhesion of the nanocomposite.

  20. One pot synthesized Li, Zr doped porous silica nanoparticle for low temperature CO2 adsorption

    Directory of Open Access Journals (Sweden)

    Mani Ganesh

    2017-05-01

    Full Text Available Li, Zr doped porous silica was synthesized in one pot and investigated for low temperature CO2 adsorption. The synthesized nanoparticle was characterized by X-ray diffraction (XRD, N2 adsorption–desorption measurement, thermogravimetric analysis (TGA and scanning electron microscopy (SEM. The specific surface area, average pore diameter and pore volume were determined to be 962 m2/g, 2.3 nm and 0.56 cm3/g respectively. ICP-AES analysis revealed a metal content of 4 wt.% (Zr and 3.42 wt.% (Li. Their CO2 adsorption capacity was tested at room temperature and atmospheric pressure. An uptake of about 5 wt.% was observed and regenerable at a low temperature of 200 °C. This adsorption and desorption temperature of the sorbent is lower than the reported lithium silicate. The CO2 adsorption–desorption cyclic performance studies illustrated that Li, Zr doped porous silica is a recyclable, selective and potential sorbent for CO2 adsorption.

  1. Green One-pot Synthesis of Novel Polysubstituted Pyrazole Derivatives as Potential Antimicrobial Agents.

    Science.gov (United States)

    Beyzaei, Hamid; Motraghi, Zahra; Aryan, Reza; Zahedi, Mohammad Mehdi; Samzadeh-Kermani, Alireza

    2017-12-01

    Various biological properties of natural and synthetic pyrazole derivatives such as anti-inflammatory, antimicrobial, neuroprotective, anticonvulsant, antidepressant and anticancer activities encouraged us to propose a new, fast, green and eco-friendly procedure for the preparation of some novel 5-amino-3-(aryl substituted)-1-(2,4-dinitrophenyl)-1H-pyrazole-4-carbonitriles. They were efficiently synthesized via one-pot two-step process reaction of malononitrile, 2,4-dinitrophenylhydrazine and different benzaldehydes in deep eutectic solvent (DES) glycerol/potassium carbonate. The products yield and reaction times were considerably improved in the presence of applied DES. Antibacterial effects of all newly synthesized pyrazoles in comparison with several common antibiotics were evaluated against a variety of Gram-positive and Gram-negative pathogenic bacteria. In addition to, their inhibitory activities on three fungi were compared to some current antifungal agents. The moderate to good antimicrobial potentials particularly against fungi were observed in the major heterocyclic compounds according to the IZD, MIC, MBC and MFC results.

  2. One-Pot Synthesis of Waterborne Polymeric Dispersions Stabilized with Alkali-Soluble Resins

    Directory of Open Access Journals (Sweden)

    Massimo Bandiera

    2018-01-01

    Full Text Available Alkali-soluble resins (ASRs are a type of electrosteric emulsifiers of high interest because they can profitably improve the features of waterborne dispersions. In this work, they have been synthesized in-situ through a one-pot approach and they have been used as polymeric surfactants for a second emulsion polymerization step in the same reactor. This strategy provides some advantages compared to other polymerization techniques, like the intensification of the process and the absence of organic solvents. Their use can also further reduce the environmental impact of formulations for film-forming applications, since grafting reactions with the particles have been observed and quantified in relation with the synthetic parameters. These chemical linkages with the particles may reduce the leaching and the release of surfactants from polymeric films, for example in water-based coatings or adhesives. The systems have been also studied from the kinetics point of view, finding relevant differences with other electrosterically stabilized processes from the literature, as well as concerns the nucleation mechanism.

  3. One-pot, bioinspired coatings to reduce the flammability of flexible polyurethane foams.

    Science.gov (United States)

    Davis, Rick; Li, Yu-Chin; Gervasio, Michelle; Luu, Jason; Kim, Yeon Seok

    2015-03-25

    In this manuscript, natural materials were combined into a single "pot" to produce flexible, highly fire resistant, and bioinspired coatings on flexible polyurethane foam (PUF). In one step, PUF was coated with a fire protective layer constructed of a polysaccharide binder (starch or agar), a boron fire retardant (boric acid or derivative), and a dirt char former (montmorillonite clay). Nearly all coatings produced a 63% reduction in a critical flammability value, the peak heat release rate (PHRR). One formulation produced a 75% reduction in PHRR. This technology was validated in full-scale furniture fire tests, where a 75% reduction in PHRR was measured. At these PHRR values, this technology could reduce the fire threat of furniture from significant fire damage in and beyond the room of fire origin to being contained to the burning furniture. This flammability reduction was caused by three mechanisms-the gas-phase and condensed-phase processes of the boron fire retardant and the condensed-phase process of the clay. We describe the one-pot coating process and the impact of the coating composition on flammability.

  4. Rapid, one-pot synthesis of highly-soluble carbon nanotubes functionalized by L-arginine

    Science.gov (United States)

    Ghiadi, Behnam; Baniadam, Majid; Maghrebi, Morteza; Amiri, Ahmad

    2013-04-01

    Functionalization of carbon nanotubes (CNTs) is a necessary step to exploit their valuable properties. Due to having several steps and especially acid treatment, most of current methods of functionalization result in irrecoverable defects on CNTs structure. Here, multiwalled carbon nanotubes (MWCNTs) were functionalized with L-arginine in a simple, one-pot and rapid microwave-assisted technique without any acid treatment step. The CNT functionalities were analyzed with infrared spectroscopy, thermogravimetric analysis, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy. The results confirmed the covalent functionalization of L-arginine with very low defects on CNTs. Also it is found that increase of input powers of microwave in the range 500-900 W, monotonically increase the degree of functionalization. The maximum dispersibility of MWCNT was found ˜1.03 mg/mL corresponding to 900 W irradiation. Accounting considerable low treatment time, the method may be applied for large-scale solubilization of MWCNTs in an industrial scale.

  5. On Metal Segregation of Bimetallic Nanocatalysts Prepared by a One-Pot Method in Microemulsions

    Directory of Open Access Journals (Sweden)

    Concha Tojo

    2017-02-01

    Full Text Available A comparative study on different bimetallic nanocatalysts prepared from microemulsions using a one-pot method has been carried out. The analysis of experimental observations, complemented by simulation studies, provides detailed insight into the factors affecting nanoparticle architecture: (1 The metal segregation in a bimetallic nanocatalysts is the result of the combination of three main kinetic parameters: the reduction rate of metal precursors (related to reduction standard potentials, the material intermicellar exchange rate (determined by microemulsion composition, and the metal precursors concentration; (2 A minimum difference between the reduction standard potentials of the two metals of 0.20 V is needed to obtain a core-shell structure. For values ∆ε0 smaller than 0.20 V the obtaining of alloys cannot be avoided, neither by changing the microemulsion nor by increasing metal concentration; (3 As a rule, the higher the film flexibility around the micelles, the higher the degree of mixture in the nanocatalyst; (4 A minimum concentration of metal precursors is required to get a core-shell structure. This minimum concentration depends on the microemulsion flexibility and on the difference in reduction rates.

  6. One-pot synthesis of silanol-free nanosized MFI zeolite

    Science.gov (United States)

    Grand, Julien; Talapaneni, Siddulu Naidu; Vicente, Aurélie; Fernandez, Christian; Dib, Eddy; Aleksandrov, Hristiyan A.; Vayssilov, Georgi N.; Retoux, Richard; Boullay, Philippe; Gilson, Jean-Pierre; Valtchev, Valentin; Mintova, Svetlana

    2017-10-01

    The synthesis of nanostructured zeolites enables modification of catalytically relevant properties such as effective surface area and diffusion path length. Nanostructured zeolites may be synthesized either in alkaline media, and so contain significant numbers of hydrophilic silanol groups, or in expensive and harmful fluoride-containing media. Here, we report and characterize, using a combination of experimental and theoretical techniques, the one-pot synthesis of silanol-free nanosized MFI-type zeolites by introducing atomically dispersed tungsten; this prevents silanol group occurrence by forming flexible W-O-Si bridges. These W-O-Si bonds are more stable than Si-O-Si in the all-silica MFI zeolite. Tungsten incorporation in nanosized MFI crystals also modifies other properties such as structural features, hydrophobicity and Lewis acidity. The effect of these is illustrated on the catalytic epoxidation of styrene and separation of CO2 and NO2. Silanol-free nanosized W-MFI zeolites open new perspectives for catalytic and separation applications.

  7. One pot phytosynthesis of gold nanoparticles using Genipa americana fruit extract and its biological applications

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Brajesh, E-mail: krmbraj@gmail.com [Centro de Nanociencia y Nanotecnologia, Universidad de las Fuerzas Armadas ESPE, Av. Gral. Rumiñahui s/n, Sangolqui, P.O. BOX 171-5-231B (Ecuador); Smita, Kumari; Cumbal, Luis [Centro de Nanociencia y Nanotecnologia, Universidad de las Fuerzas Armadas ESPE, Av. Gral. Rumiñahui s/n, Sangolqui, P.O. BOX 171-5-231B (Ecuador); Camacho, Javier [Centro de Nanociencia y Nanotecnologia, Universidad de las Fuerzas Armadas ESPE, Av. Gral. Rumiñahui s/n, Sangolqui, P.O. BOX 171-5-231B (Ecuador); Centro de Investigación y de Estudios Avanzados del Instituto Politécnico Nacional, Departamento de Farmacología, C.P. 07360 Mexico City (Mexico); Hernández-Gallegos, Elisabeth; Guadalupe Chávez-López, María de [Centro de Investigación y de Estudios Avanzados del Instituto Politécnico Nacional, Departamento de Farmacología, C.P. 07360 Mexico City (Mexico); Grijalva, Marcelo; Andrade, Kleber [Centro de Nanociencia y Nanotecnologia, Universidad de las Fuerzas Armadas ESPE, Av. Gral. Rumiñahui s/n, Sangolqui, P.O. BOX 171-5-231B (Ecuador)

    2016-05-01

    In this article, rapid one pot synthesis of gold nanoparticles (GNPs) using an eco-friendly extract of Genipa americana L. fruit is described. Electrospray ionization mass spectrometry (ESI-MS) and Fourier transform infrared (FTIR) spectroscopic studies demonstrated that small molecules such as genipin, genipaol, geniposide and ranolazine can act as reducer as well as stabilizers. The monodispersed, spherical GNPs were further characterized by UV–vis spectroscopy at λ{sub max} = 535 nm, transmission electron microscopy (TEM), dynamic light scattering (DLS) and X-ray diffraction (XRD) analysis. This synthetic approach offers a greener and alternate route to the preparation of GNPs free from toxic chemical components and stable for 6–7 months under room temperature. The green synthesized GNPs showed weak antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl and no cytotoxicity against A-549 and HeLa human cancer cell lines, from lung and cervix. This study opens a new industrial scope of G. americana fruit in nanoscience and as surface modified GNPs can be developed into a successful drug carrier for future pharmaceutical products. - Highlights: • Gold nanoparticles can be synthesized by Genipa americana fruit extract. • TEM-DLS analysis confirmed that the average particle size is 30.4 ± 14.9 nm. • Nanoparticles showed weak antioxidant and no cytotoxicity activity.

  8. Preparing hydrophobic nanocellulose-silica film by a facile one-pot method.

    Science.gov (United States)

    Le, Duy; Kongparakul, Suwadee; Samart, Chanatip; Phanthong, Patchiya; Karnjanakom, Surachai; Abudula, Abuliti; Guan, Guoqing

    2016-11-20

    Hydrophobic nanocellulose-silica film was successfully prepared by a facile one-pot method using tetraethoxysilane (TEOS) and dodecyl triethoxylsilane (DTES). Morphological characterization of the hydrophobic nanocellulose-silica (NC-SiO2-DTES) film showed well self-assembled DTES modified silica spherical nanoparticles with the particle sizes in the range of 88-126nm over the nanocellulose film. The hydrophobicity of the NC-SiO2-DTES film was achieved owing to the improvement of roughness of the nanocellulose film by coating dodecyl- terminated silica nanoparticles. An increase in DTES loading amount and reaction time increased the hydrophobicity of the film, and the optimum condition for NC-SiO2-DTES film preparation was achieved at DTES/TEOS molar ratio of 2.0 for 8h reaction time. Besides, the NC-SiO2-DTES film performed superoleophilic property with octane and hexadecane contact angles of 0°. It also showed an excellent hydrophobic property over all pH values ranged from 1 to 14. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. One-pot fabrication and antimicrobial properties of novel PET nonwoven fabrics

    International Nuclear Information System (INIS)

    Lin Song; Wang Zheng; Qi Jiancheng; Wu Jinhui; Tian Tao; Hao Limei; Yang Jingquan; Hou Lili

    2011-01-01

    Recently, with the ever-growing demand for healthy living, more and more research is focused on materials capable of killing harmful microorganisms around the world. It is believed that designing such protective materials for hygienic and biomedical applications can benefit people in professional areas and daily life. Thus, in this paper, one novel kind of antibacterial poly(ethylene terephthalate) (PET) nonwoven fabrics was conveniently one-pot prepared, with the combined immobilization of two biological antimicrobial agents, i.e. ε-polylysine and natamycin, by using the soft methacrylate nonwoven fabrics adhesives. Then, the antimicrobial activities of the functional fabrics were investigated by using the standard shaking-flask method, showing excellent antibacterial efficiency (AE) against both Escherichia coli (8099) and Staphylococcus aureus (ATCC 6538) (AE > 99.99%) compared with untreated PET nonwoven fabrics. The anti-bioaerosol tests also showed similar trends. Meantime, scanning electron microscopy analysis indicated that the bacteria on the antibacterial PET appeared to be partly bacteriolyzed and showed much less viability than those on the pristine ones. Moreover, the long residual biocidal action of such modified PET fabrics was also evaluated, and the antibacterial activity of antibacterial fibers was unaffected by the 3 month artificially accelerated aging.

  10. Acid, silver, and solvent-free gold-catalyzed hydrophenoxylation of internal alkynes

    Directory of Open Access Journals (Sweden)

    Marcia E. Richard

    2013-10-01

    Full Text Available A range of arylgold compounds have been synthesized and investigated as single-component catalysts for the hydrophenoxylation of unactivated internal alkynes. Both carbene and phosphine-ligated compounds were screened as part of this work, and the most efficient catalysts contained either JohnPhos or IPr/SIPr. Phenols bearing either electron-withdrawing or electron-donating groups were efficiently added using these catalysts. No silver salts, acids, or solvents were needed for the catalysis, and either microwave or conventional heating afforded moderate to excellent yields of the vinyl ethers.

  11. Monoglycerides and Diglycerides Synthesis in a Solvent-Free System by Lipase-Catalyzed Glycerolysis

    Science.gov (United States)

    Fregolente, Patricia Bogalhos Lucente; Fregolente, Leonardo Vasconcelos; Pinto, Gláucia Maria F.; Batistella, Benedito César; Wolf-Maciel, Maria Regina; Filho, Rubens Maciel

    Five lipases were screened (Thermomyces lanuginosus free and immobilized forms, Candida antarctica B, Candida rugosa, Aspergillus niger, and Rhizomucor miehei) to study their ability to produce monoglycerides (MG) and diglycerides (DG) through enzymatic glycerolysis of soybean oil. Lipase from C. antarctica was further studied to verify the enzyme load (wt% of oil mass), the molar ratio glycerol/oil, and the water content (wt% of glycerol) on the glycerolysis reaction. The best DG and MG productions were in the range 45-48% and 28-30% (w/w, based on the total oil), respectively. Using immobilized lipases, the amount of free fatty acids (FFA) produced was about 5%. However, the amount of FFA produced when using free lipases, with 3.5% extra water in the system, is equivalent to the MG yield, about 23%. The extra water content provides a competition between hydrolysis and glycerolysis reactions, increasing the FFA production.

  12. One-pot reverse microemulsion synthesis of core-shell structured YVO4:Eu3+@SiO2 nanocomposites

    Science.gov (United States)

    Liu, Lina; Yue, Surong; Zhang, Yongsheng; Qin, Ruifei; Liu, Lishuang; Zhang, Dongmei; Sun, Ruirui; Chen, Linfeng

    2015-01-01

    Core-shell structured YVO4:Eu3+@SiO2 nanocomposite particles were synthesized using a one-pot reverse microemulsion method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV absorption spectra, and photoluminescent spectra. The nanocomposite particles are well-dispersed and about 20 nm in average size. The synthesis method is of one-pot, simplifying the preparation of this kind of core-shell structured nanocomposites. The formation process of these nanocomposite particles is suggested and the photoluminescence properties of them are studied and compared with those of uncoated YVO4:Eu3+ sample.

  13. Solvent-free Oxidation of Alcohols and Mild Catalytic Deprotection of ...

    African Journals Online (AJOL)

    tetrabromobenzene- 1,3-disulphonamide (TBBDA) can be used for solvent-free oxidation of primary and secondary alcohols to the corresponding carbonyl compounds without over-oxidation, and efficient catalytic deprotection of various silyl ...

  14. Solvent-free Oxidation of Alcohols and Mild Catalytic Deprotection of ...

    African Journals Online (AJOL)

    NJD

    tetrabromobenzene-1,3-disulphonamide. (TBBDA) can be used for solvent-free oxidation of primary and secondary alcohols to the corresponding carbonyl compounds without over-oxidation, and efficient catalytic deprotection of various silyl ...

  15. Microwave-assisted silica-promoted solvent-free synthesis of ...

    Indian Academy of Sciences (India)

    assisted silica-promoted solvent-free synthesis ... Author Affiliations. G Krishnamurthy1 K V Jagannath1. Department of Studies in Chemistry, Central College Campus, Bangalore University, Dr. B R Ambedkar Veedhi, Bengalore 560 001, India ...

  16. Solvent Free Preparation of p-Cymene from Limonene Using Vietnamese Montmorillonite

    DEFF Research Database (Denmark)

    Nguyen, Thao-Tran Thi; Duus, Fritz; Le, Thach Ngoc

    2013-01-01

    p-Cymene, an important intermediate in industrial chemistry, has been prepared in good yields by thermally induced dehydrogenation of limonene under solvent-free reaction conditions using Vietnamese montmorillonite as an efficient green catalyst.......p-Cymene, an important intermediate in industrial chemistry, has been prepared in good yields by thermally induced dehydrogenation of limonene under solvent-free reaction conditions using Vietnamese montmorillonite as an efficient green catalyst....

  17. One-pot synthesis of Au@SiO2 catalysts: A click chemistry approach

    KAUST Repository

    Solovyeva, Vera A.

    2014-10-13

    Using the copper-catalyzed azide-alkyne cycloaddition "click" reaction, a library of triazole amphiphiles with a variety of functional polar "heads" and hydrophobic or superhydrophobic "tails" was synthesized. The amphiphiles were evaluated for their ability to stabilize small Au nanoparticles, and, at the same time, serve as templates for nanocasting porous SiO2. One of the Au@SiO2 materials thus prepared was found to be a highly active catalyst for the Au nanoparticle-catalyzed regioselective hydroamination of alkynes.

  18. Chain-growth click polymerization of AB2 monomers for the formation of hyperbranched polymers with low polydispersities in a one-pot process.

    Science.gov (United States)

    Shi, Yi; Graff, Robert W; Cao, Xiaosong; Wang, Xiaofeng; Gao, Haifeng

    2015-06-22

    Hyperbranched polymers are important soft nanomaterials but robust synthetic methods with which the polymer structures can be easily controlled have rarely been reported. For the first time, we present a one-pot one-batch synthesis of polytriazole-based hyperbranched polymers with both low polydispersity and a high degree of branching (DB) using a copper-catalyzed azide-alkyne cycloaddition (CuAAC) polymerization. The use of a trifunctional AB2 monomer that contains one alkyne and two azide groups ensures that all Cu catalysts are bound to polytriazole polymers at low monomer conversion. Subsequent CuAAC polymerization displayed the features of a "living" chain-growth mechanism with a linear increase in molecular weight with conversion and clean chain extension for repeated monomer additions. Furthermore, the triazole group in a linear (L) monomer unit complexed Cu(I) , which catalyzed a faster reaction of the second azide group to quickly convert the L unit into a dendritic unit, producing hyperbranched polymers with DB=0.83. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. One-pot synthesis and characterization of rhodamine derivative-loaded magnetic core–shell nanoparticles

    International Nuclear Information System (INIS)

    Zhang Jin; Li Jiaxin; Razavi, Fereidoon S.; Mumin, Abdul Md.

    2011-01-01

    A new method to produce elaborate nanostructure with magnetic and fluorescent properties in one entity is reported in this article. Magnetite (Fe 3 O 4 ) coated with fluorescent silica (SiO 2 ) shell was produced through the one-pot reaction, in which one reactor was utilized to realize the synthesis of superparamagnetic core of Fe 3 O 4 , the formation of SiO 2 coating through the condensation and polymerization of tetraethylorthosilicate (TEOS), and the encapsulation of tetramethyl rhodamine isothiocyanate-dextran (TRITC-dextran) within silica shell. Transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, and X-ray diffraction (XRD) were carried out to investigate the core–shell structure. The magnetic core of the core–shell nanoparticles is 60 ± 10 nm in diameter. The thickness of the fluorescent SiO 2 shell is estimated at 15 ± 5 nm. In addition, the fluorescent signal of the SiO 2 shell has been detected by the laser confocal scanning microscopy (LCSM) with emission wavelength (λ em ) at 566 nm. In addition, the magnetic properties of TRITC-dextran loaded silica-coating iron oxide nanoparticles (Fe 3 O 4 -SiO 2 NPs) were studied. The hysteresis loop of the core–shell NPs measured at room temperature shows that the saturation magnetization (M s ) is not reached even at the field of 70 kOe (7T). Meanwhile, the very low coercivity (H c ) and remanent magnetization (M r ) are 0.375 kOe and 6.6 emu/g, respectively, at room temperature. It indicates that the core–shell particles have the superparamagnetic properties. The measured blocking temperature (T B ) of the TRITC-dextran loaded Fe 3 O 4 -SiO 2 NPs is about 122.5 K. It is expected that the multifunctional core–shell nanoparticles can be used in bio-imaging.

  20. One-pot integrated biofuel production using low-cost biocompatible protic ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Jian; Konda, Murthy; Parthasarathi, Ramakrishnan; Dutta, Tanmoy; Valiev, Marat; Xu, Feng; Simmons, Blake A.; Singh, Seema

    2017-01-01

    The transformation of biomass into liquid fuels is of great importance. Previous work has demonstrated the capability of specific ionic liquids (ILs), such as 1-ethyl-3-methylimidazolium acetate ([C(2)C(1)Im][OAc]) and cholinium lysinate ([Ch][Lys]), to be effective biomass pretreatment solvents. Using these ILs for an integrated biomass-to-biofuel configuration is still challenging due to a significant water-wash related to the high toxicity of [C(2)C(1)Im][OAc] and pH adjustment prior to saccharification for the highly basic [Ch][Lys]. In this work, we demonstrate, for the first time, that a one-pot integrated biofuel production is enabled by a low cost (similar to$1 per kg) and biocompatible protic IL (PIL), ethanolamine acetate, without pH adjustments, water-wash and solid-liquid separations. After pretreatment, the whole slurry is directly used for simultaneous saccharification and fermentation (SSF) with commercial enzyme cocktails and wild type yeast strains, generating 70% of the theoretical ethanol yield (based on switchgrass). The structure-performance relationships of PILs in terms of lignin removal, net basicity, and pH value are systematically studied. A technoeconomic analysis (TEA) revealed that an integrated biorefinery concept based on this PIL process could potentially reduce the minimum ethanol selling price by more than 40% compared to scenarios that require pH adjustment prior to SSF. Improvement of the economic performance will be made by reducing the dilution and enzyme loading during SSF as identified by TEA. This study demonstrates the impact of a biocompatible IL in terms of process optimization and conversion efficiency, and opens up avenues for realizing an IL based efficiently integrated biomass conversion technology.

  1. Preparation of glycosyl thiourea derivatives from glycosyl azides using sulfamic acid and sodium iodide in one-pot.

    Science.gov (United States)

    Gucchait, Arin; Jana, Manas; Jana, Kuladip; Misra, Anup Kumar

    2016-11-03

    Novel one-pot reaction conditions have been developed for the preparation of glycosyl thiourea derivatives directly from glycosyl azides mediated by a combination of sulfamic acid and sodium iodide. The reaction conditions were clean, non-toxic and the products were isolated in good to excellent yield. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Base-Free, One-Pot Chemocatalytic Conversion of Glycerol to Methyl Lactate using Supported Gold Catalysts

    NARCIS (Netherlands)

    Pazhavelikkakath Purushothaman, Rajeesh Kumar; van Haveren, Jacco; Melian Cabrera, Ignacio; van Eck, Ernst R.H.; Heeres, Hero J.

    We report an efficient one-pot conversion of glycerol (GLY) to methyl lactate (MLACT) in methanol in good yields (73% at 95% GLY conversion) by using Au nanoparticles on commercially available ultra-stable zeolite-Y (USY) as the catalyst (160 degrees C, air, 47bar pressure, 0.25M GLY, GLY-to-Au mol

  3. Base-Free, One-Pot Chemocatalytic Conversion of Glycerol to Methyl Lactate using Supported Gold Catalysts

    NARCIS (Netherlands)

    Purushothaman, R.K.P.; Haveren, van J.; Melian-Cabrera, I.; Eck, van E.R.H.; Heeres, H.J.

    2014-01-01

    We report an efficient one-pot conversion of glycerol (GLY) to methyl lactate (MLACT) in methanol in good yields (73% at 95% GLY conversion) by using Au nanoparticles on commercially available ultra-stable zeolite-Y (USY) as the catalyst (160 degrees C, air, 47bar pressure, 0.25M GLY, GLY-to-Au mol

  4. Synthesis of Quaternary Ammonium Salts of Tricyclic Cationic Drugs: A One-Pot Synthesis for the Bioorganic Chemistry Laboratory

    Science.gov (United States)

    Brunauer, Linda S.; Mogannam, Abid C.; Hwee, Won B.; Chen, James Y.

    2007-01-01

    A one-pot conversion of tricyclic cationic drugs to their quaternary ammonium forms is described for a widely used bioactive drug: chlorpromazine, a phenothiazine-based antipsychotic. After conversion to its free base, the parent drug was methylated using substoichiometric amounts of methyl iodide dissolved in ether; the charged quaternary…

  5. One-pot synthesis of water soluble iron nanoparticles using rationally-designed peptides and ligand release.

    Science.gov (United States)

    Papst, Stefanie; Cheong, Soshan; Banholzer, Moritz J; Brimble, Margaret A; Williams, David E; Tilley, Richard D

    2013-05-18

    Herein we report the rational design of new phosphopeptides for control of nucleation, growth and aggregation of water-soluble, superparamagnetic iron-iron oxide core-shell nanoparticles. The use of the designed peptides enables a one-pot synthesis that avoids utilizing unstable or toxic iron precursors, organic solvents, and the need for exchange of capping agent after synthesis of the NPs.

  6. One-Pot Catalyst-Free Synthesis of β- and γ-Hydroxy Sulfides using Diaryliodonium Salts and Microwave Irradiation

    Science.gov (United States)

    A facile one-pot high-yield protocol is described for the preparation of β- and γ-hydroxy sulfides directly from diaryliodonium salts, potassium thiocyanate, and ethane-1,2-diol (ethylene glycol)/propane-1,3-diol (β-propylene glycol) without the need for any additional catalyst o...

  7. One-pot preparation of unsaturated polyester nanocomposites containing functionalized graphene sheets via a novel solvent-exchange method

    Science.gov (United States)

    This paper reports a convenient one-pot method integrating a novel solvent-exchange method into in situ melt polycondensation to fabricate unsaturated polyester nanocomposites containing functionalized graphene sheets (FGS). A novel solvent-exchange method was first developed to prepare graphene oxi...

  8. Ultrasound Promoted Green and Facile One-Pot Multicomponent Synthesis of 3,4-dihydropyrano[c]chromene Derivatives

    Directory of Open Access Journals (Sweden)

    Ravikumar Nagalapalli

    2013-01-01

    Full Text Available Ultrasound promoted mild one-pot multicomponent synthesis of 3,4-dihydropyrano[c]chromenes from 4-hydroxycoumarin, arylaldehydes and malononitrile was achieved in aqueous media. The methodology promises advantages of short reaction times, environmentally benign conditions, high yields, and operational convenience.

  9. Ultrasound Promoted Green and Facile One-Pot Multicomponent Synthesis of 3,4-dihydropyrano[c]chromene Derivatives

    OpenAIRE

    Nagalapalli, Ravikumar; Jaggavarapu, Satyanarayana Reddy; Jalli, Venkata Prasad; Kamalakaran, Anand Solomon; Gaddamanugu, Gopikrishna

    2013-01-01

    Ultrasound promoted mild one-pot multicomponent synthesis of 3,4-dihydropyrano[c]chromenes from 4-hydroxycoumarin, arylaldehydes and malononitrile was achieved in aqueous media. The methodology promises advantages of short reaction times, environmentally benign conditions, high yields, and operational convenience.

  10. A one-pot regioselective synthesis of benzo[d]imidazo[2,1-b]thiazoles.

    Science.gov (United States)

    Zhang, Xinhai; Jia, Jiong; Ma, Chen

    2012-10-21

    Benzo[d]imidazo[2,1-b]thiazole analogues were synthesized via a one-pot metal-free procedure. A series of benzene and pyridine substrates were employed to the methodology. The desired products were generated in moderate to good yields. The effect of substituent group had also been studied.

  11. Synthesis of non-natural carbohydrates from glycerol and aldehydes in a one-pot four-enzyme cascade reaction

    NARCIS (Netherlands)

    Babich, L.; Hartog, L.; Falcicchio, P.; Oost, van der J.

    2011-01-01

    A simple procedure has been developed for the synthesis of enantio- and diastereomerically pure carbohydrate analogues from glycerol and a variety of aldehydes in one pot using a four-enzyme cascade reaction. As a proof of concept of the usefulness of this enzymatic catalytic cascade the naturally

  12. Mechanistic investigation of the one-pot formation of amides by oxidative coupling of alcohols with amines in methanol

    DEFF Research Database (Denmark)

    Mielby, Jerrik Jørgen; Riisager, Anders; Fristrup, Peter

    2013-01-01

    The one-pot formation of amides by oxidative coupling of alcohols and amines via intermediate formation of methyl ester using supported gold and base as catalysts was studied using the Hammett methodology. Determining the relative reactivity of four different para-substituted benzyl alcohol deriv...... a theoretical Hammett plot that was in good agreement with the one obtained experimentally....

  13. A Biocatalytic One-Pot Approach for the Preparation of Lignin Oligomers Using an Oxidase/Peroxidase Cascade Enzyme System

    NARCIS (Netherlands)

    Habib, Mohamed H. M.; Deuss, Peter J.; Loncar, Nikola; Trajkovic, Milos; Fraaije, Marco W.

    2017-01-01

    Synthetic lignin was prepared biocatalytically in a one-pot, two-step reaction using an oxidase/peroxidase cascade enzyme system. Using eugenol in combination with eugenol oxidase and a peroxidase, lignin-like material was produced. The cascade reaction takes advantage of the ability of the oxidase

  14. Stereo- and regio-selective one-pot synthesis of triazole-based unnatural amino acids and β- amino triazoles

    Science.gov (United States)

    Synthesis of triazole based unnatural amino acids and β-amino triazole has been described via stereo and regioselective one-pot multi-component reaction of sulfamidates, sodium azide, and alkynes under MW conditions. The developed method is applicable to a broad substrate scope a...

  15. Highly luminescent CdSe/ZnSe core-shell quantum dots of one-pot preparation in octadecene

    NARCIS (Netherlands)

    Zeng, Q.; Kong, X.; Zhang, Y.; Zhang, H.

    2008-01-01

    CdSe/ZnSe core-shell quantum dots were synthesized using a new one-pot procedure where the core was prepared in octadecene. A ZnSe shell around a CdSe nanoparticle was formed by the reaction of selenium-richness on the surfaces of CdSe nanoparticles with Zn2+ from the injected zinc stearate

  16. Solvent-free and time-efficient Suzuki-Miyaura reaction in a ball mill: the solid reagent system KF-Al(2)O(3) under inspection.

    Science.gov (United States)

    Bernhardt, Franziska; Trotzki, Ronald; Szuppa, Tony; Stolle, Achim; Ondruschka, Bernd

    2010-01-22

    Although a plethora of synthetic procedures mediated by KF-loaded aluminas is available in the literature, there is almost no data concerning the influence of parameters such as alumina modification or KF-loading on experimental results. Hence, the Pd-catalyzed, solvent-free Suzuki-Miyaura reaction was chosen as model reaction to investigate the effect of the above mentioned parameters on the results of coupling reactions. The results from ball milling experiments led to the conclusion that self-prepared and commercially available KF-Al₂O ₃differ in water content. The higher the residual water content, the higher are the product yields.

  17. A thermoresponsive nanorattle containing two different catalysts for controllable one-pot tandem catalysis

    Science.gov (United States)

    Niu, Chengrong; Hu, Jie; Li, Yinfeng; Leng, Jinghang; Li, Songjun

    2018-03-01

    In the present work, a thermoresponsive nanorattle with a Ag nanoparticle (NP) core (one catalyst in the nanorattle), and a poly(N-isopropylacrylamide) shell was developed. An imidazole group was grafted on the polymer shell by copolymerization as the other catalyst. Owing to the catalytic activities of the imidazole group and Ag NP with regards to hydrolysis and reduction, respectively, this nanorattle exhibited tandem-reaction catalytic abilities. In addition, because of the shrinkage of the poly(N-isopropylacrylamide) shell at high temperatures, the tandem reaction could be controlled to stop at the first reaction step. That is to say, only the hydrolysis reaction was catalyzed by the imidazole group being grafted on the surface of the shell. The reduction step in the tandem reaction catalyzed by the Ag particle, however, was switched off by the shrinkage of the poly(N-isopropylacrylamide) shell. This protocol opens up an opportunity to develop controllable catalysts for complicated chemical processes.

  18. One-pot synthesis and characterization of rhodamine derivative-loaded magnetic core-shell nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Jin, E-mail: jzhang@eng.uwo.ca; Li Jiaxin [University of Western Ontario, Department of Chemical and Biochemical Engineering (Canada); Razavi, Fereidoon S. [Brock University, Department of Physics (Canada); Mumin, Abdul Md. [University of Western Ontario, Department of Chemical and Biochemical Engineering (Canada)

    2011-05-15

    A new method to produce elaborate nanostructure with magnetic and fluorescent properties in one entity is reported in this article. Magnetite (Fe{sub 3}O{sub 4}) coated with fluorescent silica (SiO{sub 2}) shell was produced through the one-pot reaction, in which one reactor was utilized to realize the synthesis of superparamagnetic core of Fe{sub 3}O{sub 4}, the formation of SiO{sub 2} coating through the condensation and polymerization of tetraethylorthosilicate (TEOS), and the encapsulation of tetramethyl rhodamine isothiocyanate-dextran (TRITC-dextran) within silica shell. Transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, and X-ray diffraction (XRD) were carried out to investigate the core-shell structure. The magnetic core of the core-shell nanoparticles is 60 {+-} 10 nm in diameter. The thickness of the fluorescent SiO{sub 2} shell is estimated at 15 {+-} 5 nm. In addition, the fluorescent signal of the SiO{sub 2} shell has been detected by the laser confocal scanning microscopy (LCSM) with emission wavelength ({lambda}{sub em}) at 566 nm. In addition, the magnetic properties of TRITC-dextran loaded silica-coating iron oxide nanoparticles (Fe{sub 3}O{sub 4}-SiO{sub 2} NPs) were studied. The hysteresis loop of the core-shell NPs measured at room temperature shows that the saturation magnetization (M{sub s}) is not reached even at the field of 70 kOe (7T). Meanwhile, the very low coercivity (H{sub c}) and remanent magnetization (M{sub r}) are 0.375 kOe and 6.6 emu/g, respectively, at room temperature. It indicates that the core-shell particles have the superparamagnetic properties. The measured blocking temperature (T{sub B}) of the TRITC-dextran loaded Fe{sub 3}O{sub 4}-SiO{sub 2} NPs is about 122.5 K. It is expected that the multifunctional core-shell nanoparticles can be used in bio-imaging.

  19. One-pot growth of two-dimensional lateral heterostructures via sequential edge-epitaxy.

    Science.gov (United States)

    Sahoo, Prasana K; Memaran, Shahriar; Xin, Yan; Balicas, Luis; Gutiérrez, Humberto R

    2018-01-03

    Two-dimensional heterojunctions of transition-metal dichalcogenides have great potential for application in low-power, high-performance and flexible electro-optical devices, such as tunnelling transistors, light-emitting diodes, photodetectors and photovoltaic cells. Although complex heterostructures have been fabricated via the van der Waals stacking of different two-dimensional materials, the in situ fabrication of high-quality lateral heterostructures with multiple junctions remains a challenge. Transition-metal-dichalcogenide lateral heterostructures have been synthesized via single-step, two-step or multi-step growth processes. However, these methods lack the flexibility to control, in situ, the growth of individual domains. In situ synthesis of multi-junction lateral heterostructures does not require multiple exchanges of sources or reactors, a limitation in previous approaches as it exposes the edges to ambient contamination, compromises the homogeneity of domain size in periodic structures, and results in long processing times. Here we report a one-pot synthetic approach, using a single heterogeneous solid source, for the continuous fabrication of lateral multi-junction heterostructures consisting of monolayers of transition-metal dichalcogenides. The sequential formation of heterojunctions is achieved solely by changing the composition of the reactive gas environment in the presence of water vapour. This enables selective control of the water-induced oxidation and volatilization of each transition-metal precursor, as well as its nucleation on the substrate, leading to sequential edge-epitaxy of distinct transition-metal dichalcogenides. Photoluminescence maps confirm the sequential spatial modulation of the bandgap, and atomic-resolution images reveal defect-free lateral connectivity between the different transition-metal-dichalcogenide domains within a single crystal structure. Electrical transport measurements revealed diode-like responses across the

  20. One-pot growth of two-dimensional lateral heterostructures via sequential edge-epitaxy

    Science.gov (United States)

    Sahoo, Prasana K.; Memaran, Shahriar; Xin, Yan; Balicas, Luis; Gutiérrez, Humberto R.

    2018-01-01

    Two-dimensional heterojunctions of transition-metal dichalcogenides have great potential for application in low-power, high-performance and flexible electro-optical devices, such as tunnelling transistors, light-emitting diodes, photodetectors and photovoltaic cells. Although complex heterostructures have been fabricated via the van der Waals stacking of different two-dimensional materials, the in situ fabrication of high-quality lateral heterostructures with multiple junctions remains a challenge. Transition-metal-dichalcogenide lateral heterostructures have been synthesized via single-step, two-step or multi-step growth processes. However, these methods lack the flexibility to control, in situ, the growth of individual domains. In situ synthesis of multi-junction lateral heterostructures does not require multiple exchanges of sources or reactors, a limitation in previous approaches as it exposes the edges to ambient contamination, compromises the homogeneity of domain size in periodic structures, and results in long processing times. Here we report a one-pot synthetic approach, using a single heterogeneous solid source, for the continuous fabrication of lateral multi-junction heterostructures consisting of monolayers of transition-metal dichalcogenides. The sequential formation of heterojunctions is achieved solely by changing the composition of the reactive gas environment in the presence of water vapour. This enables selective control of the water-induced oxidation and volatilization of each transition-metal precursor, as well as its nucleation on the substrate, leading to sequential edge-epitaxy of distinct transition-metal dichalcogenides. Photoluminescence maps confirm the sequential spatial modulation of the bandgap, and atomic-resolution images reveal defect-free lateral connectivity between the different transition-metal-dichalcogenide domains within a single crystal structure. Electrical transport measurements revealed diode-like responses across the

  1. Synthesis of task specific and reusable protic ionic liquids for one-pot multicomponent syntheses

    Science.gov (United States)

    Sardar, Sabahat; Wilfred, Cecilia Devi; Marc, Leveque Jean

    2016-11-01

    Protic ionic liquids (ILs) synthesized from 1-methylimidazole with 1,3-propane sultone and 1,4-butane sultone catalyzed Mannich reaction at 25 °C to afford Mannich bases in high yield (76%) and less time duration (20 min). Ionic liquids have been used as dual reagent i.e., as catalyst as well as solvent. Simple extraction by water separated ionic liquid from reaction mixture with 4 times recycling without any significant loss in activity.

  2. Zr(HSO{sub 4}){sub 4} as an efficient catalyst for the preparation of 10-aryl-6,8-dimethyl-6,10dihydro-5-oxa-6,8-diazaanthra[2,3-d][1,3]dioxole-7 ,9-diones under solvent-free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jiangli [Xinxiang Medical University, Xinxiang, Henan (China). Dept. Psychology of the Second Affiliated; Li, Wei Lin; Wu, Li Qiang [Xinxiang Medical University, Xinxiang, Henan (China). School of Pharmacy

    2011-07-01

    A one-pot three-component condensation of 3,4-methylenedioxyphenol, aromatic aldehydes, and 1,3-dimethylbarbituric acid, efficiently promoted in the presence of Zr(HSO{sub 4}){sub 4} under solvent free conditions, produced 10-aryl-6,8-dimethyl-6,10-dihydro-5-oxa-6,8-diazaanthra[2,3-d][1,3] dioxole-7,9-diones. The method offers several advantages including simple, easy and clean work-up procedure, relatively short reaction times and good to high yields of the products. (author)

  3. Direct Production of Furfural in One-pot Fashion from Raw Biomass Using Brønsted Acidic Ionic Liquids.

    Science.gov (United States)

    Matsagar, Babasaheb M; Hossain, Shahriar A; Islam, Tofazzal; Alamri, Hatem R; Alothman, Zeid A; Yamauchi, Yusuke; Dhepe, Paresh L; Wu, Kevin C-W

    2017-10-18

    The conversion of raw biomass into C5-sugars and furfural was demonstrated with the one-pot method using Brønsted acidic ionic liquids (BAILs) without any mineral acids or metal halides. Various BAILs were synthesized and characterized using NMR, FT-IR, TGA, and CHNS microanalysis and were used as the catalyst for raw biomass conversion. The remarkably high yield (i.e. 88%) of C5 sugars from bagasse can be obtained using 1-methyl-3(3-sulfopropyl)-imidazolium hydrogen sulfate ([C 3 SO 3 HMIM][HSO 4 ]) BAIL catalyst in a water medium. Similarly, the [C 3 SO 3 HMIM][HSO 4 ] BAIL also converts the bagasse into furfural with very high yield (73%) in one-pot method using a water/toluene biphasic solvent system.

  4. One-pot synthesis of enantiomerically pure N-protected allylic amines from N-protected α-amino esters

    Directory of Open Access Journals (Sweden)

    Gastón Silveira-Dorta

    2016-05-01

    Full Text Available An improved protocol for the synthesis of enantiomerically pure allylic amines is reported. N-Protected α-amino esters derived from natural amino acids were submitted to a one-pot tandem reduction–olefination process. The sequential reduction with DIBAL-H at −78 °C and subsequent in situ addition of organophosphorus reagents yielded the corresponding allylic amines without the need to isolate the intermediate aldehyde. This circumvents the problem of instability of the aldehydes. The method tolerates well both Wittig and Horner–Wadsworth–Emmons organophosphorus reagents. A better Z-(diastereoselectivity was observed when compared to the previous one-pot method. The (diastereoselectivity of the process was affected neither by the reaction solvent nor by the amount of DIBAL-H employed. The method is compatible with the presence of free hydroxy groups as shown with serine and threonine derivatives.

  5. Post-modified acid-base bifunctional MIL-101(Cr) for one-pot deacetalization-Knoevenagel reaction

    Energy Technology Data Exchange (ETDEWEB)

    Mu, Manman [Tianjin University, School of Science (China); Yan, Xilong; Li, Yang; Chen, Ligong, E-mail: lgchen@tju.edu.cn [Collaborative Innovation Center of Chemical Science and Engineering (Tianjin) (China)

    2017-04-15

    A novel and convenient approach for the construction of the bifunctional MIL-101 material bearing sulfonic acid and amino groups was established via the post-synthetic modification. This material possesses high BET surface area (1446 m{sup 2}/g) and large pore volume (0.77 cm{sup 3}/g). Significantly, this material could serve as a bifunctional heterogeneous catalyst and was initially employed for one-pot deacetalization-Knoevenagel reaction, exhibiting excellent catalytic performance (yield 99.74%). More importantly, it can be easily recovered and reused at least three times. Finally, our proposed catalytic mechanism indicated that amino and the sulfonic acid groups played a synergistic effect on this one-pot deacetalization-Knoevenagel reaction.

  6. Combining silver catalysis and organocatalysis: a sequential Michael addition/hydroalkoxylation one-pot approach to annulated coumarins.

    Science.gov (United States)

    Hack, Daniel; Chauhan, Pankaj; Deckers, Kristina; Hermann, Gary N; Mertens, Lucas; Raabe, Gerhard; Enders, Dieter

    2014-10-03

    A highly stereoselective one-pot procedure for the synthesis of five-membered annulated hydroxycoumarins has been developed. By merging primary amine catalysis with silver catalysis, a series of functionalized coumarin derivatives were obtained in good yields (up to 91%) and good to excellent enantioselectivities (up to 99% ee) via a Michael addition/hydroalkoxylation reaction. Depending on the substituents on the enynone, the synthesis of annulated six-membered rings is also feasible.

  7. One pot obtention of a tetrabutylammonium hydroxide solution for ironporphyrin-OH- interaction studies in organic solvents

    Directory of Open Access Journals (Sweden)

    Lídia S. Iwamoto

    1999-04-01

    Full Text Available In this work we report the obtention of a tetrabutylammonium hydroxide (TBAOH solution in acetonitrile in a one pot process in order to study the interaction ironporphyrinOH- in non-aqueous systems. All the reactions were carried out under dry argon atmosphere to prevent the contamination of the solution with CO2, which leads to the formation of (TBA2CO3.

  8. A one-pot synthesis of reduced graphene oxide-Cu₂S quantum dot hybrids for optoelectronic devices.

    Science.gov (United States)

    Su, Yanjie; Lu, Xiaonan; Xie, Minmin; Geng, Huijuan; Wei, Hao; Yang, Zhi; Zhang, Yafei

    2013-10-07

    We demonstrate a facile one-pot approach for the synthesis of reduced graphene oxide (rGO)-cuprous sulfide quantum dot (Cu₂S QD) hybrids, wherein the reduction of GO and the growth of Cu₂S QDs on graphene occur simultaneously. The as-synthesized rGO-Cu₂S QD hybrids exhibit an excellent photoelectric response and efficient electron transfer from the Cu₂S QDs to the rGO sheets.

  9. One-Pot Synthesis of (+)-Nootkatone via Dark Singlet Oxygenation of Valencene: The Triple Role of the Amphiphilic Molybdate Catalyst

    OpenAIRE

    Bing Hong; Raphaël Lebeuf; Stéphanie Delbaere; Paul L. Alsters; Véronique Nardello-Rataj

    2016-01-01

    Efficient one-pot catalytic synthesis of (+)-nootkatone was performed from (+)-valencene using only hydrogen peroxide and amphiphilic molybdate ions. The process required no solvent and proceeded in three cascade reactions: (i) singlet oxygenation of valencene according to the ene reaction; (ii) Schenck rearrangement of one hydroperoxide into the secondary β-hydroperoxide; and (iii) dehydration of the hydroperoxide into the desired (+)-nootkatone. The solvent effect on the hydroperoxide rearr...

  10. Continuous one-pot synthesis of sandwich structured core-shell particles and transformation to yolk-shell particles.

    Science.gov (United States)

    Ko, You Na; Kang, Yun Chan; Park, Seung Bin

    2013-05-10

    Scalable continuous ultrasonic spray pyrolysis is used to develop a facile one-pot method of synthesizing sandwich structured core-shell particles consisting of a Pd core, a V2O5 inner layer, and a porous SiO2 outer layer. Pd@SiO2 yolk-shell particles are easily formed by removing the V2O5 inner layer.

  11. One-pot functionalisation of N-substituted tetrahydroisoquinolines by photooxidation and tunable organometallic trapping of iminium intermediates.

    Science.gov (United States)

    Barham, Joshua P; John, Matthew P; Murphy, John A

    2014-01-01

    Nucleophilic trapping of iminium salts generated via oxidative functionalisation of tertiary amines is well established with stabilised carbon nucleophiles. The few reports of organometallic additions have limited scope of substrate and organometallic nucleophile. We report a novel, one-pot methodology that functionalises N-substituted tetrahydroisoquinolines by visible light-assisted photooxidation, followed by trapping of the resultant iminium ions with organometallic nucleophiles. This affords 1,2-disubstituted tetrahydroisoquinolines in moderate to excellent yields.

  12. The role of thiophenol in the proposed mechanism for one pot transformation of 2-phenylthio-3-aminocyclohexanols to dehydropiperidine derivatives

    Directory of Open Access Journals (Sweden)

    Firouzeh Nemati

    2016-11-01

    Full Text Available This paper describes the effect of thiophenol concentration on photochemical rearrangement of 2-phenylthio-3-aminocyclohexanols to the corresponding protected aminoaldehydes. The obtained aminoaldehyde is in equilibrium with its corresponding deoxyazasugar. The latter could be converted to the corresponding dehydropiperidine with a good yield in the same reaction media by controlling the thiophenol concentration. Also a proposed mechanism for this one pot transformation is reported.

  13. A green one-pot three-component synthesis of spirooxindoles under conventional heating conditions or microwave irradiation by using Fe3O4@SiO2-imid-PMAn magnetic porous nanospheres as a recyclable catalyst

    Science.gov (United States)

    Esmaeilpour, Mohsen; Javidi, Jaber; Divar, Masoumeh

    2017-02-01

    An efficient, green and environmentally procedure for the synthesis of spirooxindole derivatives has been developed by a one-pot three-component reaction of isatin derivatives, activated methylene, and 1,3-dicarbonyl compounds in the presence of Fe3O4@SiO2-imid-PMAn magnetic nanocatalyst under conventional heating conditions in water or microwave irradiation under solvent-free conditions. The reactions under conventional heating conditions were compared with the microwave-assisted reactions. The suggested method offers several advantages such as excellent yields, short reaction times, operational simplicity, a cleaner reaction, absence of any tedious workup or purification and ease of recovery and reusability of the catalyst by a magnetic field. In addition, the excellent catalytic performance in a water medium and the easy preparation, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. The catalyst can be easily recovered by a magnetic field and reused for six consecutive reaction cycles without significant loss of activity. Also, the morphology of Fe3O4@SiO2-imid-PMAn, particle size distribution and leaching of nano H3PMo12O40 (PMAn) after reaction cycles were investigated by scanning electron microscopy (SEM), dynamic light scattering (DLS), and inductively coupled plasma (ICP) analyzer.

  14. 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

    Energy Technology Data Exchange (ETDEWEB)

    Rostami, Amin; Tahmasbi, Bahman; Yari, Ako [Univ. of Kurdistan, Sanandaj (Iran, Islamic Republic of)

    2013-05-15

    N-Propylsulfamic acid supported onto magnetic Fe{sub 3}O{sub 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 .deg. 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.

  15. A green one-pot three-component synthesis of spirooxindoles under conventional heating conditions or microwave irradiation by using Fe{sub 3}O{sub 4}@SiO{sub 2}-imid-PMA{sup n} magnetic porous nanospheres as a recyclable catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Esmaeilpour, Mohsen, E-mail: m1250m551085@yahoo.com [Chemistry Department, College of Science, Shiraz University, Shiraz (Iran, Islamic Republic of); Javidi, Jaber, E-mail: JaberJavidi@gmail.com [Department of Pharmaceutics, School of Pharmacy, Shahid Beheshti University of Medical Sciences, Tehran (Iran, Islamic Republic of); Students Research Committee, School of Pharmacy, Shahid Beheshti University of Medical Sciences, Tehran (Iran, Islamic Republic of); Divar, Masoumeh [Chemistry Department, College of Science, Shiraz University, Shiraz (Iran, Islamic Republic of)

    2017-02-01

    An efficient, green and environmentally procedure for the synthesis of spirooxindole derivatives has been developed by a one-pot three-component reaction of isatin derivatives, activated methylene, and 1,3-dicarbonyl compounds in the presence of Fe{sub 3}O{sub 4}@SiO{sub 2}-imid-PMA{sup n} magnetic nanocatalyst under conventional heating conditions in water or microwave irradiation under solvent-free conditions. The reactions under conventional heating conditions were compared with the microwave-assisted reactions. The suggested method offers several advantages such as excellent yields, short reaction times, operational simplicity, a cleaner reaction, absence of any tedious workup or purification and ease of recovery and reusability of the catalyst by a magnetic field. In addition, the excellent catalytic performance in a water medium and the easy preparation, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. The catalyst can be easily recovered by a magnetic field and reused for six consecutive reaction cycles without significant loss of activity. Also, the morphology of Fe{sub 3}O{sub 4}@SiO{sub 2}-imid-PMA{sup n}, particle size distribution and leaching of nano H{sub 3}PMo{sub 12}O{sub 40} (PMA{sup n}) after reaction cycles were investigated by scanning electron microscopy (SEM), dynamic light scattering (DLS), and inductively coupled plasma (ICP) analyzer. - Graphical abstract: An efficient, green and environmentally procedure for the synthesis of spirooxindole derivatives has been developed by a one-pot three-component reaction of isatin derivatives, activated methylene, and 1,3-dicarbonyl compounds in the presence of Fe{sub 3}O{sub 4}@SiO{sub 2}-imid-PMA{sup n} magnetic nanocatalyst under conventional heating conditions in water or microwave irradiation under solvent-free conditions. - Highlights: • Using of Fe{sub 3}O{sub 4}@SiO{sub 2}-imid-PMA{sup n} magnetic

  16. Surface functionalization of SBA-15 by the solvent-free method

    International Nuclear Information System (INIS)

    Wang Yimeng; Zheng Yingwu; Zhu Jianhua

    2004-01-01

    A solvent-free technique was employed for fast modification of mesoporous materials. Copper, chromium and iron oxide species could be highly dispersed in SBA-15 by manually grinding the corresponding precursor salts and the host, followed by calcinations for the first time. This method is more effective to spontaneously disperse oxide species onto SBA-15 than impregnation, probably forming monolayer or submonolayer dispersion of salts or oxides. Besides, Cr(VI) species dominate in the mixing sample while Cr(III) species dominate in the impregnation one. In the temperature programmed surface reaction of nitrosamines, the sample prepared by solvent-free method showed a higher catalytic activity than the impregnation one

  17. A facile, efficient, and sustainable chitosan/CaHAp catalyst and one-pot synthesis of novel 2,6-diamino-pyran-3,5-dicarbonitriles.

    Science.gov (United States)

    Maddila, Suresh; Gangu, Kranthi Kumar; Maddila, Surya Narayana; Jonnalagadda, Sreekantha B

    2017-02-01

    A simple and versatile one-pot three-component synthetic protocol is devised for heterocycles, viz. 2,6-diamino-4-substituted-4H-pyran-3,5-dicarbonitrile derivatives, in short reaction times ([Formula: see text]30 min) at room temperature using ethanol as a solvent. This method involves the three-component reaction of malononitrile, substituted aldehydes, and cyanoacetamide catalyzed by chitosan-doped calcium hydroxyapatites (CS/CaHAps) giving good to excellent yields (86-96%). Twelve new pyran derivatives (4a-l) were synthesized and their structures were established and confirmed by different spectroscopic methods ([Formula: see text]H NMR, [Formula: see text]C NMR, [Formula: see text]N NMR, and HRMS). The heterogeneous catalyst, CS/CaHAp, was characterized by various instrumental techniques including XRD, TEM, SEM, and FT-IR and TGA spectroscopies. The catalyst was easily separable and reusable for up to six runs without any apparent loss of activity. The reported protocol has many benefits, such as ease of preparation, use of a green solvent, reduced reaction times, excellent product yields, and operational simplicity.

  18. Ligand-Assisted, One-Pot Synthesis of Rh-on-Cu Nanoscale Sea Urchins with High-Density Interfaces for Boosting CO Oxidation.

    Science.gov (United States)

    Wang, Wei; Cao, Zhenming; Liu, Kai; Chen, Jiayu; Wang, Yuanyuan; Xie, Shuifen

    2017-12-13

    Predictable synthesis of bimetallic nanocrystals with spatially controlled metal distributions offers a versatile route to the development of highly efficient nanocatalysts. Here we report a one-pot synthesis of super branched Rh-on-Cu nanoscale sea urchins (Rh-Cu NSUrs) with a high density of Cu-Rh interfaces by manipulating the ligand coordination chemistry. Structural analysis and UV-vis spectra reveal that ascorbic acid can serve as a Rh-selective coordination ligand in the nonaqueous synthesis to reverse the reduction potentials of Rh 3+ and Cu 2+ cations. The sequential reduction of Cu 2+ and then Rh 3+ cations, as well as the island epitaxial growth of Rh atoms on Cu cores, leads to the formation of Rh-on-Cu nanostructures mimicking sea urchin. The size of the Cu cores and the density of Rh branches can both be facilely regulated by tuning the mole ratio of Cu to Rh. The Cu-Rh NSUrs show enhanced activity and stability in catalyzing CO oxidation, as the intrinsic Cu-Rh interfaces can act as catalytic hot spots through a bifunctional mechanism. The Cu-Rh two-component system can separate the adsorption and activation of CO and O 2 on the Rh and Cu surfaces, respectively, accelerating the generation of CO 2 at the interfaces.

  19. Mesoporous Silica with Site-Isolated Amine and Phosphotungstic Acid Groups: A Solid Catalyst with Tunable Antagonistic Functions for One-Pot Tandem Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Shiju N. R.; Syed K.; Alberts A.; Brown D. and Rothenberg G.

    2011-09-15

    A bifunctional solid catalyst is prepared by combining acid and base functions on mesoporous silica supports. The co-existence of these functions is shown by a two-step reaction sequence in one pot. Excellent product yields, which cannot be obtained by separated acid and base functions in one pot, show the validity of our concept.

  20. Functional and Structural Analysis of Phenazine O-Methyltransferase LaPhzM from Lysobacter antibioticus OH13 and One-Pot Enzymatic Synthesis of the Antibiotic Myxin.

    Science.gov (United States)

    Jiang, Jiasong; Guiza Beltran, Daisy; Schacht, Andrew; Wright, Stephen; Zhang, Limei; Du, Liangcheng

    2018-03-12

    Myxin is a well-known antibiotic that had been used for decades. It belongs to the phenazine natural products that exhibit various biological activities, which are often dictated by the decorating groups on the heteroaromatic three-ring system. The three rings of myxin carry a number of decorations, including an unusual aromatic N5, N10-dioxide. We previously showed that phenazine 1,6-dicarboxylic acid (PDC) is the direct precursor of myxin, and two redox enzymes (LaPhzS and LaPhzNO1) catalyze the decarboxylative hydroxylation and aromatic N-oxidations of PDC to produce iodinin (1.6-dihydroxy- N5, N10-dioxide phenazine). In this work, we identified the LaPhzM gene from Lysobacter antibioticus OH13 and demonstrated that LaPhzM encodes a SAM-dependent O-methyltransferase converting iodinin to myxin. The results further showed that LaPhzM is responsible for both monomethoxy and dimethoxy formation in all phenazine compounds isolated from strain OH13. LaPhzM exhibits relaxed substrate selectivity, catalyzing O-methylation of phenazines with non-, mono-, or di- N-oxide. In addition, we demonstrated a one-pot biosynthesis of myxin by in vitro reconstitution of the three phenazine-ring decorating enzymes. Finally, we determined the X-ray crystal structure of LaPhzM with a bound cofactor at 1.4 Å resolution. The structure provided molecular insights into the activity and selectivity of the first characterized phenazine O-methyltransferase. These results will facilitate future exploitation of the thousands of phenazines as new antibiotics through metabolic engineering and chemoenzymatic syntheses.

  1. A one-pot glycerol-based additive-blended ethyl biodiesel production: a green process.

    Science.gov (United States)

    Zanin, Fabio G; Macedo, Alexandra; Archilha, Marcos Vinicios L R; Wendler, Edison P; Dos Santos, Alcindo A

    2013-09-01

    N-methyl-2-pyrrolidonium methyl sulfonate, a Brønsted acid ionic liquid, promoted the transesterification of soybean oil with ethanol giving a high quality fatty acid ethyl ester. At the end of the reaction, after distillation of excess of ethanol, spontaneous phase separation took place. While the clear upper phase corresponded to the ethyl ester, the lower phase was composed of a mixture of glycerol byproduct and the catalyst. By addition of a stoichiometric amount of appropriated reagents to the resulting mixture, a new ionic liquid-catalyzed process allows the conversion of the glycerol into less polar derivatives, and consequent migration to the ethyl esters phase. This work demonstrated that emulsion, phase separation and contamination problems were completely avoided and the glycerol could be incorporated into the biodiesel as additives in a single step. The whole process involves two renewable starting materials, ethanol and vegetable oil, allowing a total green additive-blended biodiesel production process. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. A Solvent-Free Base Liberation of a Tertiary Aminoalkyl Halide by Flow Chemistry

    DEFF Research Database (Denmark)

    Pedersen, Michael Jønch; Skovby, Tommy; Mealy, Michael J.

    2016-01-01

    A flow setup for base liberation of 3-(N,N-dimethylamino)propyl chloride hydrochloride and solvent-free separation of the resulting free base has been developed. Production in flow profits from an on-demand approach, useful for labile aminoalkyl halides. The requirement for obtaining a dry product...

  3. A Highly Efficient Solvent-Free Acetalization of Aldehydes to 1,1 ...

    African Journals Online (AJOL)

    NICO

    1,1-Diacetates, sulfonic acid functionalized silica, acetalization, solvent-free reaction, SiO2-Pr-SO3H. 1. Introduction. Protection of aldehydes is a frequently used and important method in organic chemistry. Many procedures have been developed for this aim. For the acetalization of carbonyl groups, acetic anhydride can be ...

  4. Solvent-free microwave extraction of essential oil from Melaleuca leucadendra L.

    Directory of Open Access Journals (Sweden)

    Widya Ismanto Aviarina

    2018-01-01

    Full Text Available Cajuput (Melaleuca leucadendra L. oil is one of potential commodity that provides an important role for the country’s foreign exchange but the extraction of these essential oil is still using conventional method such as hydrodistillation which takes a long time to produce essential oil with good quality. Therefore it is necessary to optimize the extraction process using a more effective and efficient method. So in this study the extraction is done using solvent-free microwave extraction method that are considered more effective and efficient than conventional methods. The optimum yield in the extraction of cajuput oil using solvent-free microwave extraction method is 1.0674%. The optimum yield is obtained on the feed to distiller (F/D ratio of 0.12 g/mL with microwave power of 400 W. In the extraction of cajuput oil using solvent-free microwave extraction method is performed first-order and second-order kinetics modelling. Based on kinetics modelling that has been done, it can be said that the second-order kinetic model (R2 = 0.9901 can be better represent experimental results of extraction of cajuput oil that using solvent-free microwave extraction method when compared with the first-order kinetic model (R2 = 0.9854.

  5. A Highly Efficient Solvent-Free Acetalization of Aldehydes to 1,1 ...

    African Journals Online (AJOL)

    1,1-Diacetates are prepared in excellent yields from aldehydes and acetic anhydride under solvent-free conditions at room temperature in short reaction times using catalytic amount of sulfonic acid functionalized silica (SiO2-Pr-SO3H) which could be easily handled and removed from the mixture of reaction. Keywords: 1 ...

  6. Preparation of Ultra-fine Calcium Carbonate by a Solvent-free ...

    African Journals Online (AJOL)

    The treatment of calcium chloride with sodium carbonate under solvent-free conditions with a supersonic airflow and at a low heating temperature leads to the synthesis of ultra-fine calcium carbonate. The reaction not only involves mild conditions, a simple operation, and high yields but also gives a high conversion rate.

  7. An Environmentally Friendly Solvent-free Synthesis of 3,4 ...

    African Journals Online (AJOL)

    Anhydrous p-aminobenzene sulphonic acid mediated solvent-free protocol is described for the synthesis of dihydropyrimidinones by the cyclocondensation of aldehydes, β-ketoesters and urea/thiourea. Yields obtained are significantly higher than those obtained utilizing classical Biginelli reaction conditions. Keywords: ...

  8. Solvent-free synthesis of nanosized hierarchical sodalite zeolite with a multi-hollow polycrystalline structure

    KAUST Repository

    Zeng, Shangjing

    2016-08-03

    A solvent-free route is developed for preparing nanoscale sodalite zeolite with a multi-hollow structure. Furthermore, the synthesis of nanosized hollow sodalite polycrystalline aggregates with a mesoporous structure and high crystallinity is investigated by adding an organosilane surfactant as a mesopore-generating agent.

  9. Solvent-Free Wittig Reaction: A Green Organic Chemistry Laboratory Experiment

    Science.gov (United States)

    Leung, Sam H.; Angel, Stephen A.

    2004-01-01

    Some Wittig reactions can be carried out by grinding the reactants in a mortar with a pestle for about 20 minutes, as per investigation. A laboratory experiment involving a solvent-free Wittig reaction that can be completed in a three-hour sophomore organic chemistry laboratory class period, are developed.

  10. Microwave-assisted silica-promoted solvent-free synthesis of ...

    Indian Academy of Sciences (India)

    Vol. 125, No. 4, July 2013, pp. 807–811. c Indian Academy of Sciences. Microwave-assisted silica-promoted solvent-free synthesis of triazoloquinazolinone and benzimidazoquinazolinones. G KRISHNAMURTHY. ∗ and K V JAGANNATH. Department of Studies in Chemistry, Central College Campus, Bangalore University,.

  11. Solvent-free porous framework resulted from 3D entanglement of 1D zigzag coordination polymer

    KAUST Repository

    Kole, Goutam Kumar Umar

    2010-01-01

    A solvent-free porous metal organic framework is constructed by the 3D entanglement of 1D zigzag coordination polymeric chains. The role of solvents and the effect of reaction conditions on such unique entanglement are addressed. © 2010 The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.

  12. One-Pot Enantiomeric Synthesis of Thiazole-Containing Amino Acids: Total Synthesis of Venturamides A and B.

    Science.gov (United States)

    Liu, Yi; He, Peng; Zhang, Yang; Zhang, Xiangyu; Liu, Jun; Du, Yuguo

    2018-04-06

    An effective one-pot procedure for enantiomerical synthesis of thiazole-containing amino acid (TCAA) has been established via a cascade disulfide cleavage/thiocarbonylation/intramolecular Staudinger reduction/aza-Wittig/oxidation reaction. Starting from the commercially available amino acid building blocks, a number of TCAAs were prepared in good yields and with excellent optical purities. This method bears features of mild reaction conditions, wide substrate adaptability, and good functional group tolerance. The power of this method was also demonstrated through the concise total synthesis of cyclic hexapeptide Venturamides A and B.

  13. One-pot Reductive Amination of carbonyl Compounds with Nitro Compounds by Transfer Hydrogenation over Co-Nxas catalyst.

    Science.gov (United States)

    Zhou, Peng; Zhang, Zehui

    2017-05-09

    A new method was developed for the synthesis of secondary amines through the one-pot reductive amination of carbonyl compounds with nitro compounds using formic acid as the hydrogen donor over a heterogeneous non-noble-metal catalyst (Co-N x /C-800-AT, generated by the pyrolysis of the cobalt phthalocyanine/silica composite at 800°C under a N 2 atmosphere and subsequent etching by HF). Both nitrogen and cobalt were of considerable importance in the transfer hydrogenation reactions with formic acid. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Controlled silver delivery by silver-cellulose nanocomposites prepared by a one-pot green synthesis assisted by microwaves

    International Nuclear Information System (INIS)

    Silva, Ana Rosa; Unali, Gianfranco

    2011-01-01

    Controlled silver release from cellulosic nanocomposites was achieved by synthesizing silver nanoparticles, under microwave heating for 1-15 min, in a one-pot, versatile and sustainable process in which microcrystalline cellulose simultaneously functions as reducing, stabilizing and supporting agent in water; chitin, starch and other cellulose derivatives could also be used as reducing, stabilizing and supporting agents for silver nanoparticles and the method was also found to be extensible to the preparation of noble metal (Au, Pt) and metal oxide nanoparticle (ZnO, Cu, CuO and Cu 2 O) nanocomposites.

  15. One-pot synthesis of silver@silica core-shell nanospheres and their application in optical limiting materials

    Science.gov (United States)

    Li, Chunfang; Wang, Chunlei; Ji, Zhaoyang; Jiang, Nengkai; Lin, Weihong; Li, Dongxiang

    2018-03-01

    Silica-coated metal nanoparticles are increasingly important for their many promising applications. A facile one-step synthesis of noble metal@silica core-shell nanospheres is necessary for their application in laser protection field. In this letter, a one-pot fabrication of silver@silica nanospheres was carried out, and then, silver nanoparticle-doped silicone rubber hybrid materials were prepared. Their optical limiting property to nanosecond laser was investigated and comparable optical limiting property with similar material involving multi-step synthesis of silica-coated metal nanoparticles was found.

  16. Green synthesis of tetrahydrobenzo[b]Pyrans by microwave assisted multi-component one-pot reactions in PEG-400.

    Science.gov (United States)

    Feng, Chun; Wang, Qiuyan; Lu, Cuifen; Yang, Guichun; Chen, Zuxing

    2012-01-01

    Polyethylene glycol is found to be a nontoxic and recyclable reaction medium for the microwave-assisted, multi-component one-pot reactions of aromatic aldehydes with ethyl-2-cyanoacetate and 1,3-cyclohexanedione or 5,5- dimethyl-1,3-cyclohexanedione in the presence of piperidine. This environmentally friendly microwave protocol offers ease of operation and enables recyclability of reaction medium and synthesis of a variety of substituted tetrahydrobenzo[b]pyran derivatives. It is an efficient, promising, and green synthetic strategy to construct tetrahydrobenzo[b]pyran skeleton.

  17. Novel one-pot process for the synthesis of ethyl 2-imino-4-methyl-2,3-dihydrothiazole-5-carboxylates

    Directory of Open Access Journals (Sweden)

    Beyzaei Hamid

    2015-01-01

    Full Text Available A facile one-pot two-step process for the synthesis of ethyl 2-imino-4-methyl-2,3-dihydrothiazole-5-carboxylates via the cyclocondensation of ethyl 2-thiocyanatoacetoacetate with a variety of hydrazine and hydrazide derivatives has been developed. Ethyl 2-thiocyanatoacetoacetate itself has been synthesized as intermediate from the reaction of ethyl 2-chloroacetoacetate with potassium thiocyanate (KSCN. The molecular structures of these newly synthesized compounds were elucidated on the basis of elemental analysis and spectral data.

  18. Organocatalytic one-pot synthesis of highly substituted pyridazines from Morita-Baylis-Hillman carbonates and diazo compounds.

    Science.gov (United States)

    Mao, Haibin; Lin, Aijun; Tang, Zhongkai; Hu, Hongwen; Zhu, Chengjian; Cheng, Yixiang

    2014-02-24

    A biologically inspired organocatalytic one-pot synthesis of highly functionalized pyridazines, which are ubiquitous structural units in a number of biologically active compounds, has been developed by starting from readily available diazo compounds and Morita-Baylis-Hillman (MBH) carbonates. Under mild reaction conditions, this synthetic route tolerated significant substrate variation to deliver a broad range of substituted products, including CF3 -substituted pyridazines derivatives. Moreover, the introduction of trifluoromethyl groups into the ring of pyridazine could be completed conveniently from 2,2,2-trifluorodiazoethane. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Conformationally superarmed S-ethyl glycosyl donors as effective building blocks for chemoselective oligosaccharide synthesis in one pot

    DEFF Research Database (Denmark)

    Bandara, Mithila D.; Yasomanee, Jagodige P.; Rath, Nigam P.

    2017-01-01

    A new series of superarmed glycosyl donors has been investigated. It was demonstrated that the S-ethyl leaving group allows for high reactivity, which is much higher than that of equally equipped S-phenyl glycosyl donors that were previously investigated by our groups. The superarmed S......-ethyl glycosyl donors equipped with a 2-O-benzoyl group gave complete β-stereoselectivity. Utility of the new glycosyl donors has been demonstrated in a one-pot one-addition oligosaccharide synthesis with all of the reaction components present from the beginning...

  20. One-pot cascade synthesis of azabicycles via the nitro-Mannich reaction and N-alkylation.

    Science.gov (United States)

    Disadee, Wannaporn; Ruchirawat, Somsak

    2018-01-31

    A one-pot, metal-free process for the synthesis of azabicycles is developed. The key transformations involved a cascade of double intramolecular cyclizations via the nitro-Mannich reaction and N-alkylation, providing various ring systems of azabicycles in yields up to 81% and an isomeric ratio of 62 : 1. This approach offers considerable advantages in terms of the handling of small molecules, the flexibility to introduce a functionalized side chain, and gives direct access to various azabicycles.

  1. Selection of DNA Aptamers for Ovarian Cancer Biomarker CA125 Using One-Pot SELEX and High-Throughput Sequencing

    Directory of Open Access Journals (Sweden)

    Delia J. Scoville

    2017-01-01

    Full Text Available CA125 is a mucin glycoprotein whose concentration in serum correlates with a woman’s risk of developing ovarian cancer and also indicates response to therapy in diagnosed patients. Accurate detection of this large, complex protein in patient samples is of great clinical relevance. We suggest that powerful new diagnostic tools may be enabled by the development of nucleic acid aptamers with affinity for CA125. Here, we report on our use of One-Pot SELEX to isolate single-stranded DNA aptamers with affinity for CA125, followed by high-throughput sequencing of the selected oligonucleotides. This data-rich approach, combined with bioinformatics tools, enabled the entire selection process to be characterized. Using fluorescence anisotropy and affinity probe capillary electrophoresis, the binding affinities of four aptamer candidates were evaluated. Two aptamers, CA125_1 and CA125_12, both without primers, were found to bind to clinically relevant concentrations of the protein target. Binding was differently influenced by the presence of Mg2+ ions, being required for binding of CA125_1 and abrogating binding of CA125_12. In conclusion, One-Pot SELEX was found to be a promising selection method that yielded DNA aptamers to a clinically important protein target.

  2. Simple one-pot aqueous synthesis of CdHgTe nanocrystals using sodium tellurite as the Te source

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Zhitao [Institute for Advanced Interdisciplinary Research in Science and Technology, East China Normal University, Shanghai (China); Luo, Chunhua [National Laboratory for Infrared Physics, Shanghai Institute of Technical Physics of the Chinese Academy of Sciences, Shanghai (China); Huang, Rong [Key Laboratory of Polar Materials and Devices, Ministry of Education, School of Information Science and Technology, East China Normal University, Shanghai (China); Wang, Yiting [Institute for Advanced Interdisciplinary Research in Science and Technology, East China Normal University, Shanghai (China); Peng, Hui, E-mail: hpeng@ee.ecnu.edu.cn [Key Laboratory of Polar Materials and Devices, Ministry of Education, School of Information Science and Technology, East China Normal University, Shanghai (China); State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University (China); Polymer Electronic Research Centre, The University of Auckland, Private Bag 92019, Auckland (New Zealand); Travas-sejdic, Jadranka [Polymer Electronic Research Centre, The University of Auckland, Private Bag 92019, Auckland (New Zealand)

    2014-09-15

    In this work, we systematically investigated the one-pot aqueous synthesis conditions of CdHgTe nanocrystals (NCs) using sodium tellurite (Na{sub 2}TeO{sub 3}) as the Te source, and found that the added content of Hg{sup 2+} and the initial pH value of reaction solutions significantly affected the photoluminescence quantum yield (PL QY) of alloyed CdHgTe NCs. When the concentration of Cd was 1.0 mmol L{sup −1}, the mole ratio of Cd/Te/Hg/MPA was 1:0.5:0.05:2.4, and the initial pH value of the reaction solution was about 8.78, the PL QY of as-prepared CdHgTe NCs was up to 45%. Characterization by HRTEM and XRD confirmed the crystalline nature of CdHgTe NCs. Compared to other synthetic approaches of CdHgTe NCs, our experimental results indicate that Na{sub 2}TeO{sub 3} could be an attractive alternative Te source to directly synthesize CdHgTe NCs in aqueous media. - Highlights: • A one-pot method was developed for the synthesis of highly luminescent CdHgTe nanocrystals (NCs). • Sodium tellurite was used as the Te source. • The quantum yield reached up to 45%. • The experimental conditions were optimized and the prepared CdHgTe NCs were characterized.

  3. A mild one-pot process for synthesising hydroxyapatite/biomolecule bone scaffolds for sustained and controlled antibiotic release

    International Nuclear Information System (INIS)

    Hess, Ulrike; Hill, Sebastian; Treccani, Laura; Rezwan, Kurosch; Streckbein, Philipp; Heiss, Christian

    2015-01-01

    The release of active molecules or the control of nosocomial infections for improved osteoinduction is ideally addressed by a bone substitute material. For this purpose, the feasibility of a mild one-pot process is probed for incorporating directly active proteins and antibiotics in a hydroxyapatite (HAp) based scaffold. The effect of two serum model proteins, bovine serum albumin (BSA) and fibrinogen (FIB), on the microstructure, on selected mechanical properties as well as on degradation behaviour and on protein release are investigated. By protein incorporation, the porosity can be adjusted between 54 and 70% especially due to the foaming ability of BSA. The addition of 5 wt% FIB doubles the biaxial flexural strength up to 6 MPa in comparison to samples without proteins (3 MPa). Protein release experiments show that a rapid release takes place within the first days (between around 3% for FIB and 38% for BSA). As a possible application for osteomyelitis treatment, vancomycin and gentamicin were subsequently added instead of proteins to study their release behaviour and their antibacterial activity, respectively. A controlled antibiotic release was observed for a period of 18 d. By varying the protein type, mixture and quantity, the mechanical strength porosity as well as the protein release and calcium solubility can be controlled. Our studies underpin the suitability of this mild one-pot process as a promising simple-to-use platform for controlled local drug release and bone treatment. (paper)

  4. A one-pot synthesis of reduced graphene oxide-Cu2S quantum dot hybrids for optoelectronic devices

    Science.gov (United States)

    Su, Yanjie; Lu, Xiaonan; Xie, Minmin; Geng, Huijuan; Wei, Hao; Yang, Zhi; Zhang, Yafei

    2013-09-01

    We demonstrate a facile one-pot approach for the synthesis of reduced graphene oxide (rGO)-cuprous sulfide quantum dot (Cu2S QD) hybrids, wherein the reduction of GO and the growth of Cu2S QDs on graphene occur simultaneously. The as-synthesized rGO-Cu2S QD hybrids exhibit an excellent photoelectric response and efficient electron transfer from the Cu2S QDs to the rGO sheets.We demonstrate a facile one-pot approach for the synthesis of reduced graphene oxide (rGO)-cuprous sulfide quantum dot (Cu2S QD) hybrids, wherein the reduction of GO and the growth of Cu2S QDs on graphene occur simultaneously. The as-synthesized rGO-Cu2S QD hybrids exhibit an excellent photoelectric response and efficient electron transfer from the Cu2S QDs to the rGO sheets. Electronic supplementary information (ESI) available: TGA curves of the GO and rGO-Cu2S QD hybrids, SEM images of the rGO-Cu2S QD hybrids with different Cu2S densities and typical I-V curves of pure Cu2S, with and without blue light irradiation. See DOI: 10.1039/c3nr02992a

  5. One-pot synthesis of magnetic hybrid materials based on ovoid-like carboxymethyl-cellulose/cetyltrimethylammonium-bromide templates

    International Nuclear Information System (INIS)

    Torres-Martínez, Nubia E.; Garza-Navarro, M.A.; Lucio-Porto, Raúl

    2013-01-01

    A novel one-pot synthetic procedure to obtain magnetic hybrid nanostructured materials (HNM), based on magnetic spinel-metal-oxide (SMO) nanoparticles stabilized in ovoid-like carboxymethyl-cellulose (CMC)/cetyltrimethylammonium-bromide (CTAB) templates, is reported. The HNM were synthesized from the controlled hydrolysis of inorganic salts of Fe (II) and Fe (III) into aqueous dissolutions of CMC and CTAB. The synthesized HNM were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy and static magnetic measurements. The experimental evidence suggests that, due to the competition between CTAB molecules and SMO nanoparticles to occupy CMC intermolecular sites nearby to its carboxylate functional groups, the size of both, SMO nanoparticles and ovoid-like CMC/CTAB templates can be tuned, varying the CTAB:SMO weight ratio. Moreover, it was found that the magnetic response of the HNM depends on the confinement degree of the SMO nanoparticles into the CMC/CTAB template. Hence, their magnetic characteristics can be adjusted controlling the size of the template, the quantity and distribution of the SMO nanoparticles within the template and their size. - Graphical abstract: Display Omitted - Highlights: • The synthesis of magnetic hybrid materials is reported. • The hybrid materials were synthesized following a novel one-pot procedure. • The magnetic nanoparticles were stabilized in ovoid-like templates. • The size of the templates was tuned adjusting nanoparticles weight content. • The magnetic properties of hybrid materials depend on the size of the template

  6. Advances in hexitol and ethylene glycol production by one-pot hydrolytic hydrogenation and hydrogenolysis of cellulose

    International Nuclear Information System (INIS)

    Li, Yuping; Liao, Yuhe; Cao, Xiaofeng; Wang, Tiejun; Ma, Longlong; Long, Jinxing; Liu, Qiying; Xua, Ying

    2015-01-01

    In this review, recent advances in the one-pot hydrolytic hydrogenation and hydrogenolysis of cellulose to value-added polyols, including hexitols (sorbitol, mannitol, and isosorbide) and 1,2-alkanediols (ethylene glycol and 1,2-propylene glycol), are summarized. Methods for the generation of H + in the first step of cellulose hydrolysis to form intermediate sugars, such as the use of soluble acids (mineral acids and heteropoly acids) and H + produced in situ from functional supports and H 2 dissociation, are classified and analyzed, considering its combination with active metals for the subsequent hydrogenation or hydrogenolysis of sugars to polyols. The interaction of non-noble metals such as nickel, bimetals, and tungsten with support materials in the catalytic conversion of intermediate sugars to hexitols and ethylene glycol is reviewed. The corresponding reaction pathways and mechanisms are discussed, including the conversion process using basic supports and solution conditions. Major challenges and promising routes are also suggested for the future development of the chemocatalytic conversion of cellulose. - Highlights: • Advances in the one-pot hydrolytic hydrogenation/hydrogenolysis of cellulose are summarized. • The interaction of non-noble metals with support materials for cellulose conversion is reviewed. • Method for the generation of in situ H + and effects of the acidic groups on supports are discussed. • Incomplete identification of intermediates/products causes mechanism complications. • Efficient conversion, separation and purification are other concerns for cellulose degrading

  7. One-pot conjugated linoleic acid production from castor oil by Rhizopus oryzae lipase and resting cells of Lactobacillus plantarum.

    Science.gov (United States)

    Khaskheli, Abid Ali; Talpur, Farah Naz; Cebeci Aydin, Aysun; Jawaid, Sana; Surhio, Muhammad Ali; Afridi, Hassan Imran

    2017-10-01

    Conjugated linoleic acid (CLA) has attracted as novel type of fatty acids having unusual health-promoting properties such as anticarcinogenic and antiobesitic effects. The present work employed castor oil as substrate for one-pot production of CLA using washed cells of Lactobacillus plantarum (L. plantarum) and lipases as catalysts. Among the screened lipases, the lipase Rhizopus oryzae (ROL) greatly assisted resting cells to produce CLA. Mass spectral analysis of the product showed that two major isomers of CLA were produced in the reaction mixture i.e. cis-9, trans-11 56.55% and trans-10, cis-12 43.45%. Optimum factors for CLA synthesis were found as substrate concentration (8 mg/mL), pH (6.5), washed cell concentration (12% w/v), and incubation time of 20 h. Hence, the combination of ROL with L. plantarum offers one pot production of CLA selectively using castor oil as a cost-effective substrate.

  8. One-pot synthesis of magnetic hybrid materials based on ovoid-like carboxymethyl-cellulose/cetyltrimethylammonium-bromide templates

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Martínez, Nubia E. [Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, San Nicolás de los Garza, 66450 Nuevo León (Mexico); Garza-Navarro, M.A., E-mail: marco.garzanr@uanl.edu.mx [Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, San Nicolás de los Garza, 66450 Nuevo León (Mexico); Universidad Autónoma de Nuevo León, Centro de Innovación, Investigación y Desarrollo en Ingeniería y Tecnología, Apodaca, 66600 Nuevo León (Mexico); Lucio-Porto, Raúl [Université de Nantes, CNRS, Institut des Matériaux Jean Rouxel (IMN), 2 rue de la Houssinière, BP32229, 44322 Nantes Cedex 3 (France); and others

    2013-09-16

    A novel one-pot synthetic procedure to obtain magnetic hybrid nanostructured materials (HNM), based on magnetic spinel-metal-oxide (SMO) nanoparticles stabilized in ovoid-like carboxymethyl-cellulose (CMC)/cetyltrimethylammonium-bromide (CTAB) templates, is reported. The HNM were synthesized from the controlled hydrolysis of inorganic salts of Fe (II) and Fe (III) into aqueous dissolutions of CMC and CTAB. The synthesized HNM were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy and static magnetic measurements. The experimental evidence suggests that, due to the competition between CTAB molecules and SMO nanoparticles to occupy CMC intermolecular sites nearby to its carboxylate functional groups, the size of both, SMO nanoparticles and ovoid-like CMC/CTAB templates can be tuned, varying the CTAB:SMO weight ratio. Moreover, it was found that the magnetic response of the HNM depends on the confinement degree of the SMO nanoparticles into the CMC/CTAB template. Hence, their magnetic characteristics can be adjusted controlling the size of the template, the quantity and distribution of the SMO nanoparticles within the template and their size. - Graphical abstract: Display Omitted - Highlights: • The synthesis of magnetic hybrid materials is reported. • The hybrid materials were synthesized following a novel one-pot procedure. • The magnetic nanoparticles were stabilized in ovoid-like templates. • The size of the templates was tuned adjusting nanoparticles weight content. • The magnetic properties of hybrid materials depend on the size of the template.

  9. One-pot transformation of cellobiose to formic acid and levulinic acid over ionic-liquid-based polyoxometalate hybrids.

    Science.gov (United States)

    Li, Kaixin; Bai, Linlu; Amaniampong, Prince Nana; Jia, Xinli; Lee, Jong-Min; Yang, Yanhui

    2014-09-01

    Currently, levulinic acid (LA) and formic acid (FA) are considered as important carbohydrates for the production of value-added chemicals. Their direct production from biomass will open up a new opportunity for the transformation of biomass resource to valuable chemicals. In this study, one-pot transformation of cellobiose into LA and FA was demonstrated, using a series of multiple-functional ionic liquid-based polyoxometalate (IL-POM) hybrids as catalytic materials. These IL-POMs not only markedly promoted the production of valuable chemicals including LA, FA and monosaccharides with high selectivities, but also provided great convenience of the recovery and the reuse of the catalytic materials in an environmentally friendly manner. Cellobiose conversion of 100%, LA selectivity of 46.3%, and FA selectivity of 26.1% were obtained at 423 K and 3 MPa for 3 h in presence of oxygen. A detailed catalytic mechanism for the one-pot transformation of cellobiose was also presented. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. One-pot synthesis of ethylenediamine-connected graphene/carbon nanotube composite material for isolation of clenbuterol from pork.

    Science.gov (United States)

    Yuan, Yanan; Jiao, Xiaoyan; Han, Yehong; Bai, Ligai; Liu, Haiyan; Qiao, Fengxia; Yan, Hongyuan

    2017-09-01

    A fluffy porous ethylenediamine-connected graphene/carbon nanotube composite (EGC), prepared by a simple and time-saving one-pot synthesis, was successfully applied as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) for the rapid extraction and determination of clenbuterol (CLB) from pork. In the one-pot synthesis, carbon nanotubes were inserted into graphene sheets and then connected with ethylenediamine through chemical modification to form a three-dimensional framework structure to prevent agglomeration of the graphene sheets. Under the optimum conditions for extraction and determination, good linearity was achieved for CLB in the range of 15.0-1000.0ngg -1 (r=0.9998) and the recoveries at three spiked levels were in the range of 92.2-96.2% with relative standard deviation ≤9.2% (n=3). In comparison with other adsorbents, including silica, NH 2 , C 18 , and Al 2 O 3 , EGC showed higher extraction and purification efficiency for CLB from pork samples. This analytical method combines excellent adsorption performance of EGC and high extraction efficiency of PT-SPE. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Flower-Like ZnO-Assisted One-Pot Encapsulation of Noble Metal Nanoparticles Supported Catalysts with ZIFs

    Science.gov (United States)

    Lin, Lu; Liu, Haiou; Zhang, Xiongfu

    2018-03-01

    Rational design of efficient approaches to fabricate MOFs-coated core-shell composites is promising but challenging. We report here the encapsulation of Pd nanoparticles (Pd NPs) supported flower-like ZnO (F-ZnO) microspheres with ZIF-8 shell through a facile strategy, in which the formation and immobilization of Pd NPs on F-ZnO supports and the subsequent growth of ZIF-8 shells over them are effectively integrated into one-pot synthetic route. Importantly, the utilization of ZnO both as support of Pd NPs and Zn2+ source of ZIF-8 is favorable for the implement of one-pot synthesis, due to its functions in anchoring Pd NPs and inducing ZIF-8 formation. Further insights into the morphological influence of zinc oxide particles on the resulting materials indicate that the flower-like microspheres with 2D nanosheets as subunits also benefit the coating of Pd NPs supported cores with ZIF-8, resulting in a well-defined core-shell catalyst. The achieved catalyst deliveries remarkable performance in terms of selectivity, anti-poisoning and recyclability in the liquid hydrogenations of alkenes.

  12. A facile route to end-functionalised polymers synthesised by SET-LRP via a one-pot reduction/thiol-ene Michael-type addition.

    Science.gov (United States)

    Syrett, Jay A; Jones, Mathew W; Haddleton, David M

    2010-10-14

    We report the facile synthesis of well defined, disulfide containing polymers via SET-LRP. A one-pot reduction/conjugation reaction enables post polymerisation modification with functional (meth)acrylates and acrylamides.

  13. Lipase-catalysed ester synthesis in solvent-free oil system: is it esterification or transesterification?

    Science.gov (United States)

    Sun, Jingcan; Yu, Bin; Curran, Philip; Liu, Shao-Quan

    2013-12-01

    Ester synthesis was carried out in a solvent-free system of lipase, coconut oil and ethanol or fusel alcohols to ascertain the reaction mechanism. During ester formation, octanoic and decanoic acids increased initially and then decreased gradually, indicating that ester production was a two-step reaction consisting of hydrolysis and esterification, rather than alcoholysis. With ethanol as the alcohol substrate, added butyric acid inhibited ester synthesis. However, when fusel alcohols were used as the alcohol substrate, no significant inhibitory effect by butyric acid was observed. Added octanoic acid did not show any adverse effect on the synthesis of corresponding esters. The results suggest that polarity of the reactants determines lipase activity. This study provides the first evidence on the mechanism of immobilised lipase-catalysed ester synthesis in a solvent-free system involving both hydrolysis and esterification. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. Solvent-Free Toner Printing of Organic Semiconductor Layer in Flexible Thin-Film Transistors

    Science.gov (United States)

    Sakai, Masatoshi; Koh, Tokuyuki; Toyoshima, Kenji; Nakamori, Kouta; Okada, Yugo; Yamauchi, Hiroshi; Sadamitsu, Yuichi; Shinamura, Shoji; Kudo, Kazuhiro

    2017-07-01

    A solvent-free printing process for printed electronics is successfully developed using toner-type patterning of organic semiconductor toner particles and the subsequent thin-film formation. These processes use the same principle as that used for laser printing. The organic thin-film transistors are prepared by electrically distributing the charged toner onto a Au electrode on a substrate film, followed by thermal lamination. The thermal lamination is effective for obtaining an oriented and crystalline thin film. Toner printing is environmentally friendly compared with other printing technologies because it is solvent free, saves materials, and enables easy recycling. In addition, this technology simultaneously enables both wide-area and high-resolution printing.

  15. Predicting the Disorder–Order Transition of Solvent-Free Nanoparticle–Organic Hybrid Materials

    KAUST Repository

    Yu, Hsiu-Yu

    2013-07-02

    The transition from a disordered to a face-centered-cubic phase in solvent-free oligomer-tethered nanoparticles is predicted using a density-functional theory for model hard spheres with tethered bead-spring oligomers. The transition occurs without a difference of volume fraction for the two phases, and the phase boundary is influenced by the loss of oligomer configurational entropy relative to an ideal random system in one phase compared with the other. When the particles are localized in the ordered phase, the cooperation of the oligomers in filling the space is hindered. Therefore, shorter oligomers feel a stronger entropic penalty in the ordered solid and favor the disordered phase. Strikingly, we found that the solvent-free system has a later transition than hard spheres for all investigated ratios of oligomer radius of gyration to particle radius. © 2013 American Chemical Society.

  16. Solvent-free preparation of co-crystals of phenazine and acridine with vanillin

    Energy Technology Data Exchange (ETDEWEB)

    Braga, Dario, E-mail: dario.braga@unibo.it [Dipartimento di Chimica ' G.Ciamician' , Universita degli studi di Bologna, Via Selmi 2, 40126 Bologna (Italy); Grepioni, Fabrizia; Maini, Lucia; Mazzeo, Paolo P.; Rubini, Katia [Dipartimento di Chimica ' G.Ciamician' , Universita degli studi di Bologna, Via Selmi 2, 40126 Bologna (Italy)

    2010-08-10

    Co-crystals of phenazine and acridine with vanillin have been obtained by solvent-free reaction or thermal treatment of the solid reactants: their structures, thermal behaviour and eutectic formation have been investigated via single crystal X-ray diffraction, differential scanning calorimetry (DSC), variable temperature X-ray powder diffraction and hot-stage microscopy (HSM). Polymorph screening of the reagents has also been carried out.

  17. Solvent-free preparation of co-crystals of phenazine and acridine with vanillin

    International Nuclear Information System (INIS)

    Braga, Dario; Grepioni, Fabrizia; Maini, Lucia; Mazzeo, Paolo P.; Rubini, Katia

    2010-01-01

    Co-crystals of phenazine and acridine with vanillin have been obtained by solvent-free reaction or thermal treatment of the solid reactants: their structures, thermal behaviour and eutectic formation have been investigated via single crystal X-ray diffraction, differential scanning calorimetry (DSC), variable temperature X-ray powder diffraction and hot-stage microscopy (HSM). Polymorph screening of the reagents has also been carried out.

  18. An Efficient, Mild and Solvent-Free Synthesis of Benzene Ring Acylated Harmalines

    Directory of Open Access Journals (Sweden)

    Sabira Begum

    2009-12-01

    Full Text Available A facile synthesis of a series of benzene ring acylated analogues of harmaline has been achieved by Friedel-Crafts acylation under solvent-free conditions at room temperature using acyl halides/acid anhydrides and AlCl3. The reaction afforded 10- and 12-acyl analogues of harmaline in good yield, along with minor quantities of N-acyl-tryptamines and 8-acyl analogues of N-acyltryptamines.

  19. Solvent-Free Synthesis of Flavour Esters through Immobilized Lipase Mediated Transesterification

    OpenAIRE

    Garlapati, Vijay Kumar; Banerjee, Rintu

    2013-01-01

    The synthesis of methyl butyrate and octyl acetate through immobilized Rhizopus oryzae NRRL 3562 lipase mediated transesterification was studied under solvent-free conditions. The effect of different transesterification variables, namely, molarity of alcohol, reaction time, temperature, agitation, addition of water, and enzyme amount on molar conversion (%) was investigated. A maximum molar conversion of 70.42% and 92.35% was obtained in a reaction time of 14 and 12 h with the transesterifica...

  20. Solvent-free, visible-light photocatalytic alcohol oxidations applying an organic photocatalyst

    Directory of Open Access Journals (Sweden)

    Martin Obst

    2016-11-01

    Full Text Available A method for the solvent-free photocatalytic conversion of solid and liquid substrates was developed, using a novel rod mill apparatus. In this setup, thin liquid films are realized which is crucial for an effective photocatalytic conversion due to the low penetration depth of light in heterogeneous systems. Several benzylic alcohols were oxidized with riboflavin tetraacetate as photocatalyst under blue light irradiation of the reaction mixture. The corresponding carbonyl compounds were obtained in moderate to good yields.

  1. Solvent-free microwave extraction of essential oil from Melaleuca leucadendra L.

    OpenAIRE

    Widya Ismanto Aviarina; Septya Kusuma Heri; Mahfud Mahfud

    2018-01-01

    Cajuput (Melaleuca leucadendra L.) oil is one of potential commodity that provides an important role for the country’s foreign exchange but the extraction of these essential oil is still using conventional method such as hydrodistillation which takes a long time to produce essential oil with good quality. Therefore it is necessary to optimize the extraction process using a more effective and efficient method. So in this study the extraction is done using solvent-free microwave extraction meth...

  2. Solvent-free, visible-light photocatalytic alcohol oxidations applying an organic photocatalyst

    OpenAIRE

    Obst, Martin; K?nig, Burkhard

    2016-01-01

    A method for the solvent-free photocatalytic conversion of solid and liquid substrates was developed, using a novel rod mill apparatus. In this setup, thin liquid films are realized which is crucial for an effective photocatalytic conversion due to the low penetration depth of light in heterogeneous systems. Several benzylic alcohols were oxidized with riboflavin tetraacetate as photocatalyst under blue light irradiation of the reaction mixture. The corresponding carbonyl compounds were obtai...

  3. Solvent-free liquid crystals and liquids based on genetically engineered supercharged polypeptides with high elasticity.

    Science.gov (United States)

    Liu, Kai; Pesce, Diego; Ma, Chao; Tuchband, Michael; Shuai, Min; Chen, Dong; Su, Juanjuan; Liu, Qing; Gerasimov, Jennifer Y; Kolbe, Anke; Zajaczkowski, Wojciech; Pisula, Wojciech; Müllen, Klaus; Clark, Noel A; Herrmann, Andreas

    2015-04-17

    A series of solvent-free elastin-like polypeptide liquid crystals and liquids are developed by electrostatic complexation of supercharged elastin-like polypeptides with surfactants. The smectic mesophases exhibit a high elasticity and the values can be easily tuned by varying the alkyl chain lengths of the surfactants or the lengths of the elastin-like polypeptides. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. One-pot bioprocess for lactic acid production from lignocellulosic agro-wastes by using ionic liquid stable Lactobacillus brevis.

    Science.gov (United States)

    Grewal, Jasneet; Khare, S K

    2018-03-01

    The lignocellulosic agro-wastes are an attractive renewable resource in biorefinery for production of value-added platform chemicals and biofuels. The study describes use of different agro-wastes as substrate for production of lactic acid, a C3-platform chemical and high demand industrial product by Lactobacillus brevis in a one-pot bioprocess. The simultaneous saccharification and co-fermentation (SSCF) process was achieved by L. brevis governed fermentation of sugars, derived from saccharification of ionic liquid pretreated feedstocks by nanoimmobilized cellulase, which was further recovered and used for consecutive cycle. The lactic acid yields of 0.22, 0.49, 0.52 g/g were obtained from cottonseed cake, wheat straw and sugarcane bagasse, respectively. The ionic liquid-tolerant L. brevis, cellulolytic reusable nanoimmobilized enzyme coupled with valorization of renewable feedstocks points towards a holistic approach for future biorefineries with sustainable production of bioproducts. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. A facile one-pot strategy for fabrication of carbon-based microwave absorbers: effects on annealing and paraffin content.

    Science.gov (United States)

    Zhang, Yanan; Quan, Bin; Liu, Wei; Liang, Xiaohui; Ji, Guangbin; Du, Youwei

    2017-07-18

    In this work, a one-pot strategy was proposed to synthesize carbon-coated Fe 3 O 4 and carbon-coated Fe 3 C via the pyrolysis of colloidal Fe 3 O 4 nanocrystals capped with oleic acid (OA) at different calcination temperatures. After exploring the microwave absorption performance of these composites, we found that carbon-coated Fe 3 C obtained at 700 °C possesses higher reflection loss (RL) and broader effective bandwidth (RL ≤ -10 dB) at low thickness. So the further investigation of the microwave absorption performance for carbon-capped Fe 3 C composites mixed with different mass percentages of paraffin was also carried out. The results demonstrated that the multi-dielectric relaxation process and better impedance matching, especially at low thickness and high frequency, contributed to the preferable microwave absorption greatly.

  6. One-pot hydrothermal synthesis of heterostructured ZnO/ZnS nanorod arrays with high ethanol-sensing properties.

    Science.gov (United States)

    Gao, Peng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Wang, Xiaona; Zhang, Guoli

    2012-04-10

    ZnO/ZnS heterostructured nanorod arrays with uniform diameter and length were synthesized from zinc substrates in a one-pot procedure by using a simple hydrothermal method. Structural characterization by HRTEM indicated that the heterostructured nanorods were composed of parallel segments of wurtzite-type ZnO and zinc-blende ZnS, with a distinct interface along the axial direction, which revealed the epitaxial relationship, ZnO (1010) and ZnS (111). The as-prepared ZnO/ZnS nanorods showed only two green emissions at around 523 nm and 576 nm. We also found that the nanorods exhibited high sensitivity to ethanol at relatively low temperatures, owing to their smaller size and structure. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. The preparation and physical properties of polysulfide-based elastomers through one-pot thiol-ene click reaction

    Directory of Open Access Journals (Sweden)

    Y. W. Quan

    2013-07-01

    Full Text Available In this paper, polysulfide-based elastomers were successfully prepared through a simple one-pot thiol-ene click reaction of the liquid polysulfide oligomer with bisphenol-A diacrylate resin. Real-time Fourier transform infrared spectroscopy (FTIR analysis showed that the molecular weight of the liquid polysulfide oligomer had no effect on mercaptan functional group conversion. The obtained elastomers continued to keep low temperature flexibility of polysulfide except Elastomer-LP3, which was due to higher content of bisphenol-A structure. All the samples had a tensile strength of over 0.7 MPa, which was comparable to that of polysulfide polymer cured by metal oxide. Moreover, the samples exhibited higher thermal stability than metal oxide cured polysulfide. This vulcanization methodology will provide a fast, efficient, and environmentally friendly approach (without metal oxides and plasticizers for preparing polysulfide elastomers.

  8. One-pot synthesis of polythiol ligand for highly bright and stable hydrophilic quantum dots toward bioconjugate formation

    Science.gov (United States)

    Dezhurov, Sergey V.; Krylsky, Dmitry V.; Rybakova, Anastasia V.; Ibragimova, Sagila A.; Gladyshev, Pavel P.; Vasiliev, Alexey A.; Morenkov, Oleg S.

    2018-03-01

    A fast and efficient one-pot synthesis of thiol-terminated poly(vinylpirrolidone-co-maleic anhydride-co-ethylene glycol dimethacrylate) based heterobifunctional polymer (PTVP) has been developed. The polymer was used for the modification of quantum dots (QDs) to prepare water soluble and stable QDs with emission quantum yield as high as 80%. Using carbodiimide method, PTVP-capped red light-emitting QDs were conjugated to model monoclonal antibodies specific to glycoprotein B (gB) of Aujeszky’s disease virus (ADV) and successfully used in the lateral flow assay (LFA) for the detection of ADV gB in biological fluids. A comparative analysis of the sensitivity of the method was carried out using three types of QDs emitting in the red and far-red region.

  9. One pot in situ growth of gold nanoparticles on amine-modified graphene oxide and their high catalytic properties

    Science.gov (United States)

    Ju, Yuyun; Li, Xi; Feng, Jie; Ma, Yanhua; Hu, Jing; Chen, Xingguo

    2014-10-01

    In this work, one pot strategy was proposed for in situ growth of Au nanoparticles (Au NPs) on the surface of amine-modified graphene oxide (GO@NH2) nanosheets. Au NPs were generated via an in situ reduction of Au3+ by Cu+ which was linked to the surface of GO@NH2 nanosheets through inorganic grafting. The initial Au NPs then served as seed for subsequent particle growth. The as-obtained GO@NH2-Au nanocomposites (GO@NH2-Au NCs) exhibited high catalytic activity for the degradation of 4-nitrophenol, which was a refractory pollutant that occur in industrial waste water. The catalytic efficiency was examined by turnover frequency (TOF). It was calculated to be 595 h-1, which was higher than that of other Au catalysts. Furthermore, the as-prepared catalyst showed high cycle stabilization during the catalytic reduction.

  10. Smiles Rearrangement Based Practical One-pot Synthesis of N-Alkyl/aryl-6-aminoquinolines from 6-Hydroxylquinoline

    International Nuclear Information System (INIS)

    Xie, Yongsheng; Vijaykumar, B. V. D.; Jang, Kiwan; Choi, Kyungmin; Shin, Dongsoo; Zuo, Hua; Yoon, Yongjin

    2013-01-01

    The C-N coupling protocol reported herein represents a convenient and practical synthesis of N-alkyl/aryl-6-aminoquinolines in a three-step one-pot manner by simple addition of 6-hydroxyquinoline and N-alkyl/aryl-2-chloroacetamides with Cs 2 CO 3 or K 2 CO 3 in DMF at 150 .deg. C via Smiles rearrangement. An electron donating substituent on the nitrogen counterpart would accelerate the rearrangement process to achieve various anilines in good yields. We currently engaged in making a chemical library including multifarious N-substituted-6-aminoquinolines, to be used in the screening for specific AChEI activity. Furthermore, this work extends the scope of preparing different heterocyclic synthons in drug design for various biological activities. Aminoquinolines and their derivatives are important chemical entities that are widely used as pro-drugs and drugs due to their antimicrobial, cytotoxic and anti-malarial activities etc

  11. Nb-Based Zeolites: Efficient bi-Functional Catalysts for the One-Pot Synthesis of Succinic Acid from Glucose

    Directory of Open Access Journals (Sweden)

    Magdi El Fergani

    2017-12-01

    Full Text Available The one-pot production of succinic acid from glucose was investigated in pure hot water as solvent using Nb (0.02 and 0.05 moles%-Beta zeolites obtained by a post-synthesis methodology. Structurally, they are comprised of residual framework Al-acid sites, extra-framework isolated Nb (V and Nb2O5 pore-encapsulated clusters. The Nb-modified Beta-zeolites acted as bi-functional catalysts in which glucose is dehydrated to levulinic acid (LA which, further, suffers an oxidation process to succinic acid (SA. After the optimization of the reaction conditions, that is, at 180 °C, 18 bar O2, and 12 h reaction time, the oxidation of glucose occurred with a selectivity to succinic acid as high as 84% for a total conversion.

  12. One pot four component sequential synthesis of hexahydroquinoline derivatives in aqueous media via enaminone intermediates: A green protocol

    Directory of Open Access Journals (Sweden)

    D. Patil

    2017-01-01

    Full Text Available A convenient green chemistry method through one pot four component tandem synthesis of hexahydroquinoline via enaminone intermediate using dimedone, ammonium acetate, aryl aldehydes and malononitrile has been described in aqueous media without the use of any external catalyst. The excess of ammonium acetate used acts as a reagent as well as catalyst. The incorporation of water as solvent along with eradication of external catalyst renders the protocol to comply with the green chemistry aspects. Shorter reaction time, high atom economy, easy work up and purification of products by non-chromatographic method are the crucial features of this methodology. The crystal structure of hexahydroquinoline basically shaped by chromatographic free selective reaction was determined by single crystal X-ray diffraction analysis.

  13. Lactic acid-mediated tandem one-pot synthesis of 2-aminothiazole derivatives: A rapid, scalable, and sustainable process

    Directory of Open Access Journals (Sweden)

    Mohan Reddy Bodireddy

    2016-12-01

    Full Text Available Environmentally benign and biodegradable lactic acid is identified as alternative solvent and catalyst for the tandem one-pot synthesis of Hantzsch 2-aminothiazole derivatives (4 from readily available aralkyl ketones (1 through in situ regioselective α-bromination using N-bromosuccinimide (2 followed by heterocyclization using thiourea (3 at 90–100°C. The major advantages of the present method include short reaction times (10–15 min, practical, simple to perform, easy work-up, good yield of products (up to 96%, productive for large-scale applications, free from apply of α-bromoketones (lachrymator as substrates, avoids column purification. Hence, the present method meets with the concepts of both Wender’s “ideal synthesis” and sustainable chemical process.

  14. One-Pot Synthesis of Hierarchical Flower-Like Pd-Cu Alloy Support on Graphene Towards Ethanol Oxidation

    Science.gov (United States)

    Zhang, Jingyi; Feng, Anni; Bai, Jie; Tan, Zhibing; Shao, Wenyao; Yang, Yang; Hong, Wenjing; Xiao, Zongyuan

    2017-09-01

    The synergetic effect of alloy and morphology of nanocatalysts play critical roles towards ethanol electrooxidation. In this work, we developed a novel electrocatalyst fabricated by one-pot synthesis of hierarchical flower-like palladium (Pd)-copper (Cu) alloy nanocatalysts supported on reduced graphene oxide (Pd-Cu(F)/RGO) for direct ethanol fuel cells. The structures of the catalysts were characterized by using scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectrometer (XPS). The as-synthesized Pd-Cu(F)/RGO nanocatalyst was found to exhibit higher electrocatalytic performances towards ethanol electrooxidation reaction in alkaline medium in contrast with RGO-supported Pd nanocatalyst and commercial Pd black catalyst in alkaline electrolyte, which could be attributed to the formation of alloy and the morphology of nanoparticles. The high performance of nanocatalyst reveals the great potential of the structure design of the supporting materials for the future fabrication of nanocatalysts.

  15. One-pot synthesis of MnO2-chitin hybrids for effective removal of methylene blue.

    Science.gov (United States)

    Dassanayake, Rohan S; Rajakaruna, Erandathi; Moussa, Hanna; Abidi, Noureddine

    2016-12-01

    Manganese dioxide (MnO 2 )-chitin-hybrid material was prepared by a facile "one-pot" synthesis method. MnO 2 -chitin hybrid was used for the effective removal of methylene blue (MB) from liquid solution as model for wastewater treatment. The hybrid obtained was characterized by field emission scanning electron microscopy and energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and thermogravimetric analysis. The effect of pH and temperature were studied. MnO 2 -chitin hybrid showed high performance for oxidative decolorization and removal of MB. Typically, 25mL of MB (20mg/L) can be completely decolorized in 2.5min with 8.5mg of the MnO 2 -chitin hybrid. The hybrid material exhibited excellent recyclability and durability with the degradation value of 99% for MB after ten consecutive cycles. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. One-pot non-enzymatic formation of firefly luciferin in a neutral buffer from p-benzoquinone and cysteine.

    Science.gov (United States)

    Kanie, Shusei; Nishikawa, Toshio; Ojika, Makoto; Oba, Yuichi

    2016-04-21

    Firefly luciferin, the substrate for the bioluminescence reaction of luminous beetles, possesses a benzothiazole ring, which is rare in nature. Here, we demonstrate a novel one-pot reaction to give firefly luciferin in a neutral buffer from p-benzoquinone and cysteine without any synthetic reagents or enzymes. The formation of firefly luciferin was low in yield in various neutral buffers, whereas it was inhibited or completely prevented in acidic or basic buffers, in organic solvents, or under a nitrogen atmosphere. Labelling analysis of the firefly luciferin using stable isotopic cysteines showed that the benzothiazole ring was formed via the decarboxylation and carbon-sulfur bond rearrangement of cysteine. These findings imply that the biosynthesis of firefly luciferin can be developed/evolved from the non-enzymatic production of firefly luciferin using common primary biosynthetic units, p-benzoquinone and cysteine.

  17. [Preparation of C18-silica hybrid monolithic capillary column by "one-pot" process and its application].

    Science.gov (United States)

    Zhang, Zhenbin; Ou, Junjie; Dong, Jing; Wang, Fangjun; Wu, Minghuo; Lin, Hui; Zou, Hanfa

    2011-09-01

    A "one-pot" process for the preparation of organic-silica hybrid capillary monolithic column by concurrently using tetramethoxysilane (TMOS), vinyltrimethoxysilane (VTMS) and the organic monomer, N-(2-(methacryloyloxy) ethyl) dimethyl-octadecylammonium bromide (MDOAB), is described. The polycondensation of alkoxysilanes and the copolymerization of MDOAB and VTMS were subsequently carried out within the confines of a capillary under the proper reaction conditions. The performance of the C18-silica hybrid monolithic column was investigated by capillary electrochromatography and capillary liquid chromatography. In addition, the C18-silica hybrid capillary monolithic column was also applied in the analysis of tryptic digests of bovine serum albumin by capillary liquid chromatography/tandem mass spectrometry (CLC-MS/MS) for demonstrating its potential in proteome analysis. This in situ process of incorporating functional groups into silica monolith provides a new way for the preparation of the organic-silica hybrid monolithic column.

  18. A simple one-pot strategy to platinum-palladium@palladium core-shell nanostructures with high electrocatalytic activity

    Science.gov (United States)

    Lv, Jing-Jing; Zheng, Jie-Ning; Wang, Ying-Ying; Wang, Ai-Jun; Chen, Li-Li; Feng, Jiu-Ju

    2014-11-01

    Well-defined platinum-palladium@palladium core-shell nanospheres (PtPd@Pd NSs) are synthesized by a facile one-pot solution approach using N-methylimidazole and poly(vinyl pyrrolidone) (PVP) as directing and capping agents, respectively, without using any seed, template, or organic solvent. The coexistence of the precursors, N-methylimidazole, PVP, and reaction temperature has great effects on the final morphology. Thus-prepared nanocomposites display an improved electrocatalytic activity for oxygen reduction reaction (ORR) in acidic media, methanol and ethylene glycol oxidation reaction in alkaline media, compared with Pt nanoparticles, Pd nanoparticles, commercial Pt black and Pd black catalysts. This method may direct a general orientation for shape control synthesis of functional bimetallic nanocrystals as promising electrocatalysts in direct alcohol fuel cells (DAFCs).

  19. One-pot synthesis of stable colloidal solutions of MFe2O4 nanoparticles using oleylamine as solvent and stabilizer

    International Nuclear Information System (INIS)

    Pérez-Mirabet, Leonardo; Solano, Eduardo; Martínez-Julián, Fernando; Guzmán, Roger; Arbiol, Jordi; Puig, Teresa; Obradors, Xavier; Pomar, Alberto; Yáñez, Ramón; Ros, Josep; Ricart, Susagna

    2013-01-01

    Highlights: ► One-pot synthesis of ferrite magnetic nanoparticles ( 3 and M(acac) 2 (M = Co, Mn, Cu and Zn) in oleylamine, which also acts as a capping ligand, by producing stable colloidal dispersions of nanoparticles in non-polar solvents. The properties of the nanoparticles have been studied via different techniques, such as transmission electron microscopy, which shows that nanoparticles are monocrystallines and a narrow dispersion in size; magnetic analyses have demonstrated that the resulting ferrite nanoparticles show high saturation values and superparamagnetic behavior at room temperature; X-ray diffraction has also been performed, and it confirms that the synthesized nanoparticles have a spinel structure. Complementarily, ligand exchange has been also carried out in order to produce dispersions of the synthesized nanoparticles in polar media

  20. Liquefaction of Biopolymers: Solvent-free Liquids and Liquid Crystals from Nucleic Acids and Proteins.

    Science.gov (United States)

    Liu, Kai; Ma, Chao; Göstl, Robert; Zhang, Lei; Herrmann, Andreas

    2017-05-16

    Biomacromolecules, such as nucleic acids, proteins, and virus particles, are persistent molecular entities with dimensions that exceed the range of their intermolecular forces hence undergoing degradation by thermally induced bond-scission upon heating. Consequently, for this type of molecule, the absence of a liquid phase can be regarded as a general phenomenon. However, certain advantageous properties usually associated with the liquid state of matter, such as processability, flowability, or molecular mobility, are highly sought-after features for biomacromolecules in a solvent-free environment. Here, we provide an overview over the design principles and synthetic pathways to obtain solvent-free liquids of biomacromolecular architectures approaching the topic from our own perspective of research. We will highlight the milestones in synthesis, including a recently developed general surfactant complexation method applicable to a large variety of biomacromolecules as well as other synthetic principles granting access to electrostatically complexed proteins and DNA. These synthetic pathways retain the function and structure of the biomacromolecules even under extreme, nonphysiological conditions at high temperatures in water-free melts challenging the existing paradigm on the role of hydration in structural biology. Under these conditions, the resulting complexes reveal their true potential for previously unthinkable applications. Moreover, these protocols open a pathway toward the assembly of anisotropic architectures, enabling the formation of solvent-free biomacromolecular thermotropic liquid crystals. These ordered biomaterials exhibit vastly different mechanical properties when compared to the individual building blocks. Beyond the preparative aspects, we will shine light on the unique potential applications and technologies resulting from solvent-free biomacromolecular fluids: From charge transport in dehydrated liquids to DNA electrochromism to biocatalysis in

  1. Development of solvent-free ambient mass spectrometry for green chemistry applications.

    Science.gov (United States)

    Liu, Pengyuan; Forni, Amanda; Chen, Hao

    2014-04-15

    Green chemistry minimizes chemical process hazards in many ways, including eliminating traditional solvents or using alternative recyclable solvents such as ionic liquids. This concept is now adopted in this study for monitoring solvent-free reactions and analysis of ionic liquids, solids, and catalysts by mass spectrometry (MS), without using any solvent. In our approach, probe electrospray ionization (PESI), an ambient ionization method, was employed for this purpose. Neat viscous room-temperature ionic liquids (RTILs) in trace amounts (e.g., 25 nL) could be directly analyzed without sample carryover effect, thereby enabling high-throughput analysis. With the probe being heated, it can also ionize ionic solid compounds such as organometallic complexes as well as a variety of neat neutral solid chemicals (e.g., amines). More importantly, moisture-sensitive samples (e.g., [bmim][AlCl4]) can be successfully ionized. Furthermore, detection of organometallic catalysts (including air-sensitive [Rh-MeDuPHOS][OTf]) in ionic liquids, a traditionally challenging task due to strong ion suppression effect from ionic liquids, can be enabled using PESI. In addition, PESI can be an ideal approach for monitoring solvent-free reactions. Using PESI-MS, we successfully examined the alkylation of amines by alcohols, the conversion of pyrylium into pyridinium, and the condensation of aldehydes with indoles as well as air- and moisture-sensitive reactions such as the oxidation of ferrocene and the condensation of pyrazoles with borohydride. Interestingly, besides the expected reaction products, the reaction intermediates such as the monopyrazolylborate ion were also observed, providing insightful information for reaction mechanisms. We believe that the presented solvent-free PESI-MS method would impact the green chemistry field.

  2. Solvent-free fabrication of thermally conductive insulating epoxy composites with boron nitride nanoplatelets as fillers.

    Science.gov (United States)

    Wang, Zifeng; Fu, Yuqiao; Meng, Wenjun; Zhi, Chunyi

    2014-01-01

    A solvent-free method for the fabrication of thermally conductive epoxy-boron nitride (BN) nanoplatelet composite material is developed in this study. By this method, polymer composites with nearly any filler fractions can be easily fabricated. The maximum thermal conductivity reaches 5.24 W/mK, which is 1,600% improvement in comparison with that of pristine epoxy material. In addition, the as-fabricated samples exhibit excellent overall performances with great mechanical property and thermal stability well preserved.

  3. One-pot synthesis and control of aqueous soluble and organic soluble carbon dots from a designable waterborne polyurethane emulsion

    Science.gov (United States)

    Gu, Jiangjiang; Hu, Donghua; Huang, Jin; Huang, Xin; Zhang, Qiuhong; Jia, Xudong; Xi, Kai

    2016-02-01

    Carbon dots (CDs) have a wide range of applications and have drawn great interest in the recent decade. The fabrication and control of CDs with different solubilities are still urgent problems for their practical use. In this paper, aqueous soluble and organic soluble CDs (ACDs, OCDs) were produced by one-pot hydrothermal treatment of a designable waterborne polyurethane (WPU) emulsion. The difference in the solubility and fluorescence of these two kinds of CDs was attributed to the various functional groups on the surface, which were derived from the different segment fragments formed by hydrothermal treatment of a block polymer. It was found that the yields of the ACDs and OCDs could be regulated by means of selecting different soft segments in WPU. The more hydrophobic soft segments could result in an increase of the OCDs and a decrease of the ACDs. While the soft segments were hydrophilic or hydrolysable under hydrothermal conditions, only ACDs were obtained. The ACDs had good fluorescence and showed low cytotoxicity for use in multicolour bio-imaging. The OCDs processed good solubility in a wide range of organic solvents and were suitable for preparing fluorescent composite films with polymers.Carbon dots (CDs) have a wide range of applications and have drawn great interest in the recent decade. The fabrication and control of CDs with different solubilities are still urgent problems for their practical use. In this paper, aqueous soluble and organic soluble CDs (ACDs, OCDs) were produced by one-pot hydrothermal treatment of a designable waterborne polyurethane (WPU) emulsion. The difference in the solubility and fluorescence of these two kinds of CDs was attributed to the various functional groups on the surface, which were derived from the different segment fragments formed by hydrothermal treatment of a block polymer. It was found that the yields of the ACDs and OCDs could be regulated by means of selecting different soft segments in WPU. The more

  4. One-pot synthesis of iniferter-bound polystyrene core nanoparticles for the controlled grafting of multilayer shells

    Science.gov (United States)

    Marchyk, Nataliya; Maximilien, Jacqueline; Beyazit, Selim; Haupt, Karsten; Sum Bui, Bernadette Tse

    2014-02-01

    A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and polymerisation time. Our method is straightforward and in addition, gives access to the preparation of fluorescent seeds and the possibility of grafting nanosized multiple shells. The core-shell nanoparticles were fully characterised by dynamic light scattering, transmission electron microscopy, Fourier transform infrared spectroscopy and microelemental analysis.A novel approach using one-pot synthesis for the production of uniform, iniferter-bound polystyrene core nanoparticles of size 30-40 nm is described. Conventional oil-in-water emulsion polymerisation of styrene and divinylbenzene, combining a hybrid initiation system (thermal and UV), triggered sequentially, was employed to form the surface-bound thiocarbamate iniferters in situ. The iniferter cores were then used as seeds for re-initiating further polymerisation by UV irradiation to produce water-compatible core-shell nanoparticles. Grafting of various shell-types is demonstrated: linear polymers of poly(N-isopropylacrylamide) brushes, crosslinked polymers bearing different surface charges and molecularly imprinted polymers. The shell thickness was readily tuned by varying the monomers' concentration and

  5. Carboxylic acid-grafted mesoporous material and its high catalytic activity in one-pot three-component coupling reaction

    Energy Technology Data Exchange (ETDEWEB)

    Gomes, Ruth; Bhaumik, Asim [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Dutta, Saikat [Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan (China)

    2014-11-01

    A new carboxylic acid functionalized mesoporous organic polymer has been synthesized via in situ radical polymerization of divinylbenzene and acrylic acid using a mesoporous silica as a seed during the polymerization process under solvothermal conditions. The mesoporous material MPDVAA-1 has been thoroughly characterized employing powder XRD, solid state {sup 13}C cross polarization magic angle spinning-nuclear magnetic resonance, FT-IR spectroscopy, N{sub 2} sorption, HR-TEM, and NH{sub 3} temperature programmed desorption-thermal conductivity detector (TPD-TCD) analysis to understand its porosity, chemical environment, bonding, and surface properties. The mesoporous polymer was used as a catalyst for a three comp onent Biginelli condensation between various aldehydes, β-keto esters, and urea/thioureas to give 3,4-dihydropyrimidine-2(1H)-ones. The reactions were carried out under conventional heating as well as solvent-free microwave irradiation of solid components, and in both the cases, the mesoporous polymer MPDVAA-1 proved to be a powerful, robust, and reusable catalyst with high catalytic efficiency.

  6. Carboxylic acid-grafted mesoporous material and its high catalytic activity in one-pot three-component coupling reaction

    Directory of Open Access Journals (Sweden)

    Ruth Gomes

    2014-11-01

    Full Text Available A new carboxylic acid functionalized mesoporous organic polymer has been synthesized via in situ radical polymerization of divinylbenzene and acrylic acid using a mesoporous silica as a seed during the polymerization process under solvothermal conditions. The mesoporous material MPDVAA-1 has been thoroughly characterized employing powder XRD, solid state 13C cross polarization magic angle spinning-nuclear magnetic resonance, FT-IR spectroscopy, N2 sorption, HR-TEM, and NH3 temperature programmed desorption-thermal conductivity detector (TPD-TCD analysis to understand its porosity, chemical environment, bonding, and surface properties. The mesoporous polymer was used as a catalyst for a three comp onent Biginelli condensation between various aldehydes, β-keto esters, and urea/thioureas to give 3,4-dihydropyrimidine-2(1H-ones. The reactions were carried out under conventional heating as well as solvent-free microwave irradiation of solid components, and in both the cases, the mesoporous polymer MPDVAA-1 proved to be a powerful, robust, and reusable catalyst with high catalytic efficiency.

  7. Synthesis of Aryl-(E)-2-(azidomethyl)alkenoate and Aryl-(Z)-2-(azidomethyl)acrylonitrile from Aryl Aldehydes and Activated Alkenes via One-Pot Way

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sang-Jin; Yang, Hae-Won; Han, Tae-Hwi; Yoon, Cheol Min [Korea University, Sejong (Korea, Republic of)

    2016-05-15

    Aryl-(E)-2-(azidomethyl)alkenoate and aryl-(Z)-2-(azidomethyl)acrylonitrile from aryl aldehydes and activated alkenes (acrylate and acrylonitrile) were synthesized in one-pot consecutive way with excellent stereoselectivity in good to high yield. The method include a three-step one-pot processes: Baylis-Hillman reaction of aryl aldehydes and activated alkenes using DABCO followed by acetylation using acetic anhydride and a catalytic amount of DMAP and nucleophilic substitution using sodium azide in DMF at room temperature. Our one-pot synthetic protocol is efficient and simple. Organoazides are one of the most important synthetic intermediates for the preparation of nitrogen-containing organic compounds, for example, amines via reduction, imines via rearrangement, and other nitrogen-containing heterocycles via cycloaddition reactions. Because allyl azides among them are versatile building skeletons for the synthesis of biologically active nitrogen-containing heterocycles, the synthesis of allyl azides have become an attractive research area.

  8. One-pot synthesis of gold nanostars using plant polyphenols for cancer photoacoustic imaging and photothermal therapy

    International Nuclear Information System (INIS)

    Zhang, Xiao-Long; Zheng, Cheng; Zhang, Yun; Yang, Huang-Hao; Liu, Xiaolong; Liu, Jingfeng

    2016-01-01

    Branched plasmonic nanostructures have been found to exhibit strong enhancement of the electromagnetic field surrounding their multi-branched petals. This feature endows them with improved performance in catalysis, surface-enhanced Raman scattering, photoacoustic imaging, and photothermal therapy. Albeit several synthesis techniques have been developed, the precisely controlled growth of highly branched nanostructures with a one-pot surfactant-free procedure is still challenging. Herein, we present a simple seedless route to synthesize gold nanostars (AuNSs) using a natural plant polyphenol, gallic acid (GA), as a reducing and stabilizing agent. The size and shape of AuNSs can be tuned by simply adjusting the amount of added GA. Under the optimum condition, the as-prepared AuNSs with diameters about 100 nm exhibit strong near-infrared absorption, good photothermal efficiency, and high biocompatibility. We demonstrate that AuNSs can be utilized for simultaneous photoacoustic imaging and photothermal therapy in living cancer cells. This study highlights facile synthesized AuNSs could serve as a promising platform for cancer diagnosis and therapy.Graphical AbstractGold nanostars (AuNSs) are synthesized by a simple seedless route using a natural plant polyphenol, gallic acid (GA), as a reducing and stabilizing agent. The AuNSs can be utilized for simultaneous photoacoustic imaging and photothermal therapy in living cancer cells. This study highlights facile synthesized AuNSs could serve as a promising platform for cancer diagnosis and therapy.

  9. Production of novel "functional oil" rich in diglycerides and phytosterol esters with "one-pot" enzymatic transesterification.

    Science.gov (United States)

    Zheng, Ming-Ming; Huang, Qing; Huang, Feng-Hong; Guo, Ping-Mei; Xiang, Xia; Deng, Qian-Chun; Li, Wen-Lin; Wan, Chu-Yun; Zheng, Chang

    2014-06-04

    Diglycerides and phytosterol esters are two important functional lipids. Phytosterol esters mixed with dietary diglyceride could not only influence body weight but also prevent or reverse insulin resistance and hyperlipidemia. In this study, a kind of novel "functional oil" rich in both diglycerides and phytosterol esters was prepared with "one-pot" enzymatic transesterification. First, lipase AYS (Candida rugosa) was immobilized on the porous cross-linked polystyrene resin beads (NKA) via hydrophobic interaction. The resulting immobilized AYS showed much better transesterification activity and thermal stability to freeways. On the basis of the excellent biocatalyst prepared, a method for high-efficiency enzymatic esterification of phytosterols with different triglycerides to produce corresponding functional oils rich in both diglycerides and phytosterol esters was developed. Four functional oils rich in both diglycerides and phytosterol esters with conversions >92.1% and controllable fatty acid composition were obtained under the optimized conditions: 80 mmol/L phytosterols, 160 mmol/L triglycerides, and 25 mg/mL AYS@NKA at 180 rpm and 50 °C for 12 h in hexane. The prepared functional oil possessed low acid value (≤1.0 mgKOH/g), peroxide value (≤2.1 mmol/kg), and conjugated diene value (≤1.96 mmol/kg) and high diglyceride and phytosterol ester contents (≥10.4 and ≥20.2%, respectively). All of the characteristics favored the wide application of the functional oil in different fields of functional food.

  10. One-pot synthesis of gold nanostars using plant polyphenols for cancer photoacoustic imaging and photothermal therapy

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiao-Long [Mengchao Hepatobiliary Hospital of Fujian Medical University, The United Innovation of Mengchao Hepatobiliary Technology Key Laboratory of Fujian Province (China); Zheng, Cheng [Fuzhou University, The Key Lab of Analysis and Detection Technology for Food Safety of the MOE, College of Chemistry (China); Zhang, Yun [Chinese Academy of Sciences, Xiamen Institute of Rare Earth Materials, Haixi Institute (China); Yang, Huang-Hao [Fuzhou University, The Key Lab of Analysis and Detection Technology for Food Safety of the MOE, College of Chemistry (China); Liu, Xiaolong, E-mail: xiaoloong.liu@gmail.com; Liu, Jingfeng, E-mail: drjingfeng@126.com [Mengchao Hepatobiliary Hospital of Fujian Medical University, The United Innovation of Mengchao Hepatobiliary Technology Key Laboratory of Fujian Province (China)

    2016-07-15

    Branched plasmonic nanostructures have been found to exhibit strong enhancement of the electromagnetic field surrounding their multi-branched petals. This feature endows them with improved performance in catalysis, surface-enhanced Raman scattering, photoacoustic imaging, and photothermal therapy. Albeit several synthesis techniques have been developed, the precisely controlled growth of highly branched nanostructures with a one-pot surfactant-free procedure is still challenging. Herein, we present a simple seedless route to synthesize gold nanostars (AuNSs) using a natural plant polyphenol, gallic acid (GA), as a reducing and stabilizing agent. The size and shape of AuNSs can be tuned by simply adjusting the amount of added GA. Under the optimum condition, the as-prepared AuNSs with diameters about 100 nm exhibit strong near-infrared absorption, good photothermal efficiency, and high biocompatibility. We demonstrate that AuNSs can be utilized for simultaneous photoacoustic imaging and photothermal therapy in living cancer cells. This study highlights facile synthesized AuNSs could serve as a promising platform for cancer diagnosis and therapy.Graphical AbstractGold nanostars (AuNSs) are synthesized by a simple seedless route using a natural plant polyphenol, gallic acid (GA), as a reducing and stabilizing agent. The AuNSs can be utilized for simultaneous photoacoustic imaging and photothermal therapy in living cancer cells. This study highlights facile synthesized AuNSs could serve as a promising platform for cancer diagnosis and therapy.

  11. Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

    Energy Technology Data Exchange (ETDEWEB)

    Martínez de Yuso, Alicia; Le Meins, Jean-Marc [Université de Strasbourg, Université de Haute-Alsace, Institut de Science des Matériaux de Mulhouse, CNRS UMR (France); Oumellal, Yassine; Paul-Boncour, Valérie; Zlotea, Claudia [Institut de Chimie et des Matériaux Paris Est, UMR 7182, CNRS-UPEC (France); Matei Ghimbeu, Camelia, E-mail: camelia.ghimbeu@uha.fr [Université de Strasbourg, Université de Haute-Alsace, Institut de Science des Matériaux de Mulhouse, CNRS UMR (France)

    2016-12-15

    An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

  12. Preparation of phenylboronic acid-silica hybrid monolithic column with one-pot approach for capillary liquid chromatography of biomolecules.

    Science.gov (United States)

    Lin, Zian; Huang, Hui; Li, Shihua; Wang, Juan; Tan, Xiaoqing; Zhang, Lan; Chen, Guonan

    2013-01-04

    A phenylboronic acid-silica hybrid monolithic column for capillary liquid chromatography (cLC) was prepared through one-pot process by using 4-vinylphenylboronic acid (VPBA) and alkoxysilanes simultaneously. The effects of the molar ratio of tetramethyloxysilane/γ-methacryloxypropyltrimethoxysilane (TMOS/γ-MAPS), amount of VPBA, and the volume of diethylene glycol (DEG) on the morphologies, permeabilities and pore properties of the prepared VPBA-silica hybrid monolithic columns were studied in detail. A relatively uniform monolithic structure with high porosity was obtained with optimized ingredients. A series of cis-diol-containing compounds, alkylbenzenes, amides, and anilines were utilized to evaluate the retention behaviors of the VPBA-silica hybrid monolithic column. The result demonstrated that the prepared VPBA-silica hybrid monolithic column exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange apart from the expected affinity interaction. The run-to-run, column-to-column and batch-to-batch reproducibility of the VPBA-silica hybrid monolith were satisfactory with the relative standard deviations (RSDs) less than 1.63% (n=5), 2.02% (n=3) and 2.90% (n=5), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the VPBA-silica hybrid monolithic column was further applied to the separation of proteins and tryptic digest of bovine serum albumin (BSA), respectively. The successful applications suggested the potential of the VPBA-silica hybrid monolith in proteome analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Continuous, One-pot Synthesis and Post-Synthetic Modification of NanoMOFs Using Droplet Nanoreactors

    Energy Technology Data Exchange (ETDEWEB)

    Jambovane, Sachin R.; Nune, Satish K.; Kelly, Ryan T.; McGrail, B. Peter; Wang, Zheming; Nandasiri, Manjula I.; Katipamula, Shanta; Trader, Cameron; Schaef, Herbert T.

    2016-11-08

    Metal-organic frameworks (MOFs); also known as porous coordination polymers (PCP) are a class of porous crystalline materials constructed by connecting metal clusters via organic linkers. The possibility of functionalization leads to virtually infinite MOF designs using generic modular methods. Functionalized MOFs can exhibit interesting physical and chemical properties including accelerated adsorption kinetics and catalysis. Although there are discrete methods to synthesize well-defined nanoscale MOFs, rapid and flexible methods are not available for continuous, one-pot synthesis and post synthesis modification (functionalization) of MOFs. Here, we show a continuous, scalable nanodroplet-based microfluidic route that not only facilitates the synthesis of MOFs at nanoscale, but also offers flexibility for direct functionalization with desired functional groups (e.g., -NH2, -COCH3, fluorescein isothiocyanate; FITC). In addition, the presented route of continuous manufacturing of functionalized MOFs takes significantly less time compared to state-of-the-art batch methods currently available (1 hr vs. several days). We envisage our approach to be a breakthrough method for synthesizing complex functionalized nanomaterials (metal, metal oxides, quantum dots and MOFs) that are not accessible by direct batch processing, and expand the range of a new class of functionalized MOF-based functional nanomaterials.

  14. One-Pot Template-Free Hydrothermal Synthesis of Monoclinic Hollow Microspheres and Their Enhanced Visible-Light Photocatalytic Activity

    Directory of Open Access Journals (Sweden)

    Bei Cheng

    2012-01-01

    Full Text Available Monoclinic-phase BiVO4 hollow microspheres with diameters of about 2–4 μm have been successfully fabricated in high yield by a one-pot template-free hydrothermal route. The reaction duration and urea concentration are shown to play important roles in the formation of the BiVO4 hollow microspheres. X-ray diffraction, scanning electron microscopy, nitrogen adsorption-desorption isotherms, fourier transform infrared spectrometry, and UV-visible diffuse reflectance spectroscopy are used to characterize the products. The results show that all the as-prepared BiVO4 samples have monoclinic phase structure and exhibit good crystallinity. A formation mechanism for the BiVO4 hollow spherical structure via a localized Ostwald ripening is proposed based on the experimental observations. In addition, studies of the photocatalytic properties by exposure to visible light irradiation demonstrate that the as-obtained BiVO4 hollow spheres show potential photocatalytic application. Hydroxyl radicals (•OH are not detected on the surface of visible-light-illuminated BiVO4 by the photoluminescence technique, suggesting that •OH is not the dominant photooxidant and photogenerated hole could directly take part in photocatalytic reaction. The prepared BiVO4 hollow spheres are also of great interest in pigment, catalysis, separation technology, biomedical engineering, and nanotechnology.

  15. One-Pot Fabrication of Dendritic NiO@carbon-nitrogen Dot Electrodes for Screening Blood Glucose Level in Diabetes.

    Science.gov (United States)

    Akhtar, Naeem; El-Safty, Sherif A; Abdelsalam, Mamdouh E; Kawarada, Hiroshi

    2015-08-21

    Selective and sensitive glucose sensors with fast response for screening diabetic blood level are demanded. In this paper, the one-pot nanoarchitecture of dendritic NiO@carbon-nitrogen (C-N) dots (designated as NCD) sphere-wrapping Ni foam electrodes are reported as an effective and sensitive glucose sensor in blood samples. In this construction design, the NCD sphere electrode with excessive surface defects, large fractions of catalytic active sites, high surface area, and mobility of electron transfer through the actively surface NCD sphere can massively enhance the electrocatalytic activity for nonenzymatic glucose detection in diabetic blood. This portable sensor enables highly sensitive recognition of glucose detection (≈0.01 × 10 -6 m) over a wider linear range (≈0.005-12 × 10 -3 m) with rapid response time of a few seconds. The key result is that the engineered NCD sphere electrodes function as simple, easy-to-use electrochemical sensing assays of glucose levels in diabetic blood patients with a wide range of precision or linearity, recyclability, and excellent selectivity, even in the presence of potentially interfering organic (ascorbic acid, uric acid, dopamine, lactose, maltose, and sucrose) and inorganic (NaCl, Na 2 SO 4 , KCl, and K 2 SO 4 ) species. The results demonstrate the potential for the electrochemical sensors to be used in preventing serious health problems associated with diabetes mismanagement. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. One-pot synthesis of powder-form {beta}-Ni(OH){sub 2} monolayer nanosheets with high electrochemical performance

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Minmin; Ren, Wanzhong; Zhao, Yunan; Liu, Yan; Cui, Hongtao, E-mail: htcui@ytu.edu.cn [Yantai University, Shandong Provincial Engineering Research Center for Light Hydrocarbon Comprehensive Utilization, College of Chemistry and Chemical Engineering (China)

    2013-08-15

    In this work, {beta}-Ni(OH){sub 2} monolayer nanosheets, which had been thought to be unachievable, were successfully prepared for the first time by a one-pot strategy using epoxide as precipitation agent and sodium dodecyl sulfate (SDS) as surfactant. The characterization results indicate that the formation of monolayer morphology depends on the mediation of SDS molecules. The XRD patterns demonstrate the loose and defective packing of Ni(OH){sub 2} layers in the SDS intercalated samples. The disappearing of vibration band of free hydroxyl groups in the FTIR spectra suggests the interlayer separation resulted by SDS. The TEM and AFM images further confirm the formation of monolayer nanosheets. It is proposed that the in situ modification of the secondary growth unit of {beta}-Ni(OH){sub 2} by SDS allows its two-dimensional anisotropic growth through steric hindrance of SDS molecules. In addition, this effect allows isolation of {beta}-Ni(OH){sub 2} from solvent with keeping of monolayer nanosheet state in dry powder. The electrochemical measurement results indicate that {beta}-Ni(OH){sub 2} monolayer nanosheets own much higher urea electrolysis performance than their corresponding multilayer structure.

  17. Flexible polyimides through one-pot synthesis as water-soluble binders for silicon anodes in lithium ion batteries

    Science.gov (United States)

    Yao, Dahua; Yang, Yu; Deng, Yonghong; Wang, Chaoyang

    2018-03-01

    A series of polyimides, which contain polyethylene glycol (PEG) segments with different molecular weight in the polymer chains, are synthesized through a facile one-pot method and characterized by Fourier transform infrared spectroscopy and hydrogen nuclear magnetic resonance spectroscopy. The main part of polyimides is originated from trimellitic anhydride chloride (TMAC) and 4,4‧-methylenedianiline, onto which PEG segments are introduced through an esterification reaction with TMAC. These obtained polyimides, which acquire excellent water solubility after being neutralized by triethylamine, are applied as water-soluble binders to silicon negative electrodes for lithium ion batteries, and significantly improve the electrochemical performance of silicon anodes. Specially, the PI-200 (polyimide copolymerized with PEG-200) based silicon electrode exhibits a high initial discharge capacity of 2989.7 mAh g-1 and remains about 2235.5 mAh g-1 after 200 cycles at the current density of 0.1 C (420 mA g-1).

  18. One-Pot Synthesis of Hyperoside by a Three-Enzyme Cascade Using a UDP-Galactose Regeneration System.

    Science.gov (United States)

    Pei, Jianjun; Chen, Anna; Zhao, Linguo; Cao, Fuliang; Ding, Gang; Xiao, Wei

    2017-07-26

    Hyperoside exhibits many biological properties and is more soluble in water than quercetin. A uridine 5'-diphosphate (UDP) galactose regeneration system and one-pot synthesis of hyperoside was described herein. Glycine max sucrose synthase (GmSUS) was coupled with Escherichia coli UDP-galactose 4-epimerase (GalE) to regenerate UDP-galactose from sucrose and UDP. Petunia hybrida glycosyltransferase (PhUGT) with high activity toward quercetin was used to synthesize hyperoside via the UDP-galactose regeneration system. The important factors for optimal synergistic catalysis were determined. Through the use of a fed-batch operation, the final titer of hyperoside increased to 2134 mg/L, with a corresponding molar conversion of 92% and maximum number of UDP-galactose regeneration cycles (RC max ) of 18.4 under optimal conditions. Therefore, the method described herein for the regeneration of UDP-galactose from UDP and sucrose can be widely used for the glycosylation of flavonoids and other bioactive substances.

  19. One-pot, one-step synthesis of 2,5-diformylfuran from carbohydrates over Mo-containing Keggin heteropolyacids.

    Science.gov (United States)

    Liu, Yu; Zhu, Liangfang; Tang, Jinqiang; Liu, Mingyang; Cheng, Ruodi; Hu, Changwei

    2014-12-01

    In this work, a one-pot strategy for directly converting fructose into 2,5-diformylfuran (DFF) over Mo-containing Keggin heteropolyacids (HPAs) in open air is developed. H3 PMo12 O40 HPA is found to show high activity and selectivity to the formation of DFF owing to its higher Brønsted acidity and moderate redox potential. The partial substitution of the H(+) in H3 PMo12 O40 with Cs(+) leads to the heterogenization of the HPA by forming its cesium salts Csx H3-x PMo12 (x=0.5, 1.5, and 2.5). A satisfactory yield of 69.3% to DFF is obtained over Cs0.5 H2.5 PMo12 polyoxometalate after deliberate optimization of the reaction conditions. The heterogenized polyoxometalate could be recycled and reused without significant loss of catalytic activity for five runs. The produced DFF could be separated from the resulting mixture by an adsorption-desorption method using activated carbon as the adsorbent and furfural as the desorbent. A highest isolated yield of 58.2% is obtained. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Green Light Emission of ZnxCd1-xSe Nanocrystals Synthesized by One-Pot Method

    Directory of Open Access Journals (Sweden)

    Shu-Ru Chung

    2013-01-01

    Full Text Available We present a facile one-pot synthesis to prepare ternary ZnxCd1-xSe (x = 0.2, 0.5, 0.8, and 1 nanocrystals (NCs with high emission quantum yield (QY, 45~89%. The effect of Zn content (x of ZnxCd1-xSe NCs on their physical properties is investigated. The NCs have a particle size of 3.2 nm and face centered cubic structure. However, the actual compositions of the NCs are Zn0.03Cd0.97Se, Zn0.11Cd0.89Se, and Zn0.38Cd0.62Se when Zn content is 0.2, 0.5, and 0.8, respectively. In terms of the optical properties, the emission wavelength shifts from 512 to 545 nm with increasing Zn content from 0 to 0.8 while the QY changes from 89 to 45, respectively. Partial replacement of Cd by Zn is beneficial to improve the QY of Zn0.2 and Zn0.5 NCs. The optical properties of ternary NCs are affected by compositional effect rather than particle size effect.

  1. Highly Efficient One-Pot Synthesis of COS-Based Block Copolymers by Using Organic Lewis Pairs.

    Science.gov (United States)

    Yang, Jia-Liang; Cao, Xiao-Han; Zhang, Cheng-Jian; Wu, Hai-Lin; Zhang, Xing-Hong

    2018-01-31

    A one-pot synthesis of block copolymer with regioregular poly(monothiocarbonate) block is described via metal-free catalysis. Lewis bases such as guanidine, quaternary onium salts, and Lewis acid triethyl borane (TEB) were equivalently combined and used as the catalysts. By using polyethylene glycol (PEG) as the macromolecular chain transfer agent (CTA), narrow polydispersity block copolymers were obtained from the copolymerization of carbonyl sulfide (COS) and propylene oxide (PO). The block copolymers had a poly(monothiocarbonate) block with perfect alternating degree and regioregularity. Unexpectedly, the addition of CTA to COS/PO copolymerization system could dramatically improve the turnover frequency (TOF) of PO (up to 240 h -1 ), higher than that of the copolymerization without CTA. In addition, the conversion of CTA could be up to 100% in most cases, as revealed by ¹H NMR spectra. Of consequence, the number-average molecular weights ( M n s) of the resultant block copolymers could be regulated by varying the feed ratio of CTA to PO. Oxygen-sulfur exchange reaction (O/S ER), which can generate randomly distributed thiocarbonate and carbonate units, was effectively suppressed in all of the cases in the presence of CTA, even at 80 °C. This work presents a versatile method for synthesizing sulfur-containing block copolymers through a metal-free route, providing an array of new block copolymers.

  2. A One Pot Synthesis of Novel Bioactive Tri-Substitute-Condensed-Imidazopyridines that Targets Snake Venom Phospholipase A2.

    Directory of Open Access Journals (Sweden)

    Nirvanappa C Anilkumar

    Full Text Available Drugs such as necopidem, saripidem, alpidem, zolpidem, and olprinone contain nitrogen-containing bicyclic, condensed-imidazo[1,2-α]pyridines as bioactive scaffolds. In this work, we report a high-yield one pot synthesis of 1-(2-methyl-8-aryl-substitued-imidazo[1,2-α]pyridin-3-ylethan-1-onefor the first-time. Subsequently, we performed in silico mode-of-action analysis and predicted that the synthesized imidazopyridines targets Phospholipase A2 (PLA2. In vitro analysis confirmed the predicted target PLA2 for the novel imidazopyridine derivative1-(2-Methyl-8-naphthalen-1-yl-imidazo [1,2-α]pyridine-3-yl-ethanone (compound 3f showing significant inhibitory activity towards snake venom PLA2 with an IC50 value of 14.3 μM. Evidently, the molecular docking analysis suggested that imidazopyridine compound was able to bind to the active site of the PLA2 with strong affinity, whose affinity values are comparable to nimesulide. Furthermore, we estimated the potential for oral bioavailability by Lipinski's Rule of Five. Hence, it is concluded that the compound 3f could be a lead molecule against snake venom PLA2.

  3. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    Directory of Open Access Journals (Sweden)

    Ezzaldeen Younes Jomma

    2016-02-01

    Full Text Available In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe3O4-PB through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe3O4-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe3O4-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM−1∙cm−2 and good long-term stability.

  4. Rapid One-Pot Microwave Synthesis of Mixed-Linker Hybrid Zeolitic-Imidazolate Framework Membranes for Tunable Gas Separations.

    Science.gov (United States)

    Hillman, Febrian; Brito, Jordan; Jeong, Hae-Kwon

    2018-02-14

    The relatively slow and complex fabrication processes of polycrystalline metal-organic framework (MOF) membranes often times restrict their way to commercialization, despite their potential for molecular separation applications. Herein, we report a rapid one-pot microwave synthesis of mixed-linker hybrid zeolitic-imidazolate framework (ZIF) membranes consisting of 2-methylimidazolate (ZIF-8 linker) and benzimidazolate (ZIF-7 linker) linkers, termed ZIF-7-8 membranes. The fast-volumetric microwave heating in conjunction with a unique counter diffusion of metal and linker solutions enabled unprecedented rapid synthesis of well-intergrown ZIF-7-8 membranes in ∼90 s, the fastest MOF membrane preparation up to date. Furthermore, we were able to tune the molecular sieving properties of the ZIF-7-8 membranes by varying the benzimidazole-to-2-methylimidazole (bIm-to-mIm) linker ratio in the hybrid frameworks. The tuning of their molecular sieving properties led to the systematic change in the permeance and selectivity of various small gases. The unprecedented rapid synthesis of well-intergrown ZIF-7-8 membranes with tunable molecular sieving properties is an important step forward for the commercial gas separation applications of ZIF membranes.

  5. One-pot synthesis of gold nanostars using plant polyphenols for cancer photoacoustic imaging and photothermal therapy

    Science.gov (United States)

    Zhang, Xiao-Long; Zheng, Cheng; Zhang, Yun; Yang, Huang-Hao; Liu, Xiaolong; Liu, Jingfeng

    2016-07-01

    Branched plasmonic nanostructures have been found to exhibit strong enhancement of the electromagnetic field surrounding their multi-branched petals. This feature endows them with improved performance in catalysis, surface-enhanced Raman scattering, photoacoustic imaging, and photothermal therapy. Albeit several synthesis techniques have been developed, the precisely controlled growth of highly branched nanostructures with a one-pot surfactant-free procedure is still challenging. Herein, we present a simple seedless route to synthesize gold nanostars (AuNSs) using a natural plant polyphenol, gallic acid (GA), as a reducing and stabilizing agent. The size and shape of AuNSs can be tuned by simply adjusting the amount of added GA. Under the optimum condition, the as-prepared AuNSs with diameters about 100 nm exhibit strong near-infrared absorption, good photothermal efficiency, and high biocompatibility. We demonstrate that AuNSs can be utilized for simultaneous photoacoustic imaging and photothermal therapy in living cancer cells. This study highlights facile synthesized AuNSs could serve as a promising platform for cancer diagnosis and therapy.

  6. One-pot synthesis and characterization of novel sodium tris(glycozirconate) and cerium glycolate precursors and their pyrolysis

    International Nuclear Information System (INIS)

    Ksapabutr, Bussarin; Gulari, Erdogan; Wongkasemjit, Sujitra

    2004-01-01

    A low-cost and facile route to the synthesis of bimetallic glycolato zirconate (Na 2 Zr(C 2 H 4 O 2 ) 3 ) and homometallic glycolato cerate (Ce(C 2 H 4 O 2 )), which can be used as alkoxide precursors for sodium zirconium oxide (and/or zirconia by sol-gel process) and ceria materials, has been developed from the reaction of inexpensive starting materials via the oxide one-pot synthesis (OOPS) process. Both complexes were directly synthesized from zirconium hydroxide/cerium hydroxide and ethylene glycol using base as catalyst. Sodium hydroxide was used in the synthesis of sodium tris(glycozirconate) complex while both triethylenetetramine (TETA) as catalyst and trace amount of sodium hydroxide as co-catalyst were used in the case of cerium glycolate complex. The structures of obtained products were investigated using FTIR, TGA, DSC, 1 H and 13 C NMR, elemental analyses, EDS and mass spectroscopy. Pyrolysis studies delineate the effects of temperature on the decomposition processes whereby sodium tris(glycozirconate) and cerium glycolate precursors transform into Na 2 O·ZrO 2 and CeO 2 , respectively. The resulting sodium zirconium oxide and ceria, after pyrolysis at 600 deg. C for 3 h, had BET surface areas of about 62 and 70 m 2 g -1 , respectively, and show monomodal pore size distributions in the mesopore region

  7. Single-step One-pot Synthesis of Graphene Foam/TiO2 Nanosheet Hybrids for Effective Water Treatment

    Science.gov (United States)

    Wang, Weilin; Wang, Zhaofeng; Liu, Jingjing; Zhang, Zhengguo; Sun, Luyi

    2017-03-01

    Millions of tons of wastewater containing both inorganic and organic pollutants are generated every day, leading to significant social, environmental, and economic issues. Herein, we designed a graphene foam/TiO2 nanosheet hybrid, which is able to effectively remove both chromium (VI) cations and organic pollutants simultaneously. This graphene foam/TiO2 nanosheet hybrid was synthesized via a facile single-step one-pot hydrothermal method. The structure of the hybrid was characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The hybrid was evaluated for both chromium (VI) and organic pollutants (using methyl blue (MB) as an example) removal, and the removal mechanism was also investigated. During water treatment, graphene and TiO2 nanosheets function complimentarily, leading to a significant synergy. The hybrid exhibited outstanding chromium (VI) and MB removal capacity, much superior to the performance of the individual pure TiO2 sheets or pure graphene foam. The hybrid could also be easily separated after water treatment, and exhibited excellent recycle stability. Considering the very facile synthesis of this graphene foam/TiO2 nanosheet hybrid, and its excellent water treatment performance and recycle stability, such a hybrid is promising for large scale production for practical applications where both chromium (VI) cations and organic dyes are the main pollutants.

  8. One-pot DNA construction for synthetic biology: the Modular Overlap-Directed Assembly with Linkers (MODAL) strategy

    Science.gov (United States)

    Casini, Arturo; MacDonald, James T.; Jonghe, Joachim De; Christodoulou, Georgia; Freemont, Paul S.; Baldwin, Geoff S.; Ellis, Tom

    2014-01-01

    Overlap-directed DNA assembly methods allow multiple DNA parts to be assembled together in one reaction. These methods, which rely on sequence homology between the ends of DNA parts, have become widely adopted in synthetic biology, despite being incompatible with a key principle of engineering: modularity. To answer this, we present MODAL: a Modular Overlap-Directed Assembly with Linkers strategy that brings modularity to overlap-directed methods, allowing assembly of an initial set of DNA parts into a variety of arrangements in one-pot reactions. MODAL is accompanied by a custom software tool that designs overlap linkers to guide assembly, allowing parts to be assembled in any specified order and orientation. The in silico design of synthetic orthogonal overlapping junctions allows for much greater efficiency in DNA assembly for a variety of different methods compared with using non-designed sequence. In tests with three different assembly technologies, the MODAL strategy gives assembly of both yeast and bacterial plasmids, composed of up to five DNA parts in the kilobase range with efficiencies of between 75 and 100%. It also seamlessly allows mutagenesis to be performed on any specified DNA parts during the process, allowing the one-step creation of construct libraries valuable for synthetic biology applications. PMID:24153110

  9. One-pot synthesis of stable water soluble Mn:ZnSe/ZnS core/shell quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Hao; Gao Xue; Liu Siyu; Su Xingguang, E-mail: suxg@jlu.edu.cn [College of Chemistry, Jilin University, Department of Analytical Chemistry (China)

    2013-06-15

    In this paper, Mn:ZnSe/ZnS core/shell-doped quantum dots (d-dots) with 3-mercaptopropionic acid as the stabilizer are successfully synthesized through a simple one-pot synthesis procedure in aqueous solution. The average diameter of Mn:ZnSe/ZnS core/shell d-dots is about 2.9 nm, which is lager than that of Mn:ZnSe cores (about 1.9 nm). The optical features and structure of the obtained Mn:ZnSe/ZnS core/shell quantum dots have been characterized by UV-Vis and fluorescence spectroscopy, X-ray diffraction, transmission electron microscopy, and X-ray photoelectron spectroscopy. The photostability against UV irradiation and chemical stability against H{sub 2}O{sub 2} etching have been studied, and the results showed that the prepared Mn:ZnSe/ZnS core/shell d-dots are more stable than CdTe quantum dots prepared in aqueous solution. Finally, the resulting core/shell quantum dots are used as fluorescent label in human osteoblast-like HepG2 cell imaging.

  10. One-Pot Fabrication of Antireflective/Antibacterial Dual-Function Ag NP-Containing Mesoporous Silica Thin Films.

    Science.gov (United States)

    Wang, Kaikai; He, Junhui

    2018-04-04

    Thin films that integrate antireflective and antibacterial dual functions are not only scientifically interesting but also highly desired in many practical applications. Unfortunately, very few studies have been devoted to the preparation of thin films with both antireflective and antibacterial properties. In this study, mesoporous silica (MSiO 2 ) thin films with uniformly dispersed Ag nanoparticles (Ag NPs) were prepared through a one-pot process, which simultaneously shows high transmittance, excellent antibacterial activity, and mechanical robustness. The optimal thin-film-coated glass substrate demonstrates a maximum transmittance of 98.8% and an average transmittance of 97.1%, respectively, in the spectral range of 400-800 nm. The growth and multiplication of typical bacteria, Escherichia coli ( E. coli), were effectively inhibited on the coated glass. Pencil hardness test, tape adhesion test, and sponge washing test showed favorable mechanical robustness with 5H pencil hardness, 5A grade adhesion, and functional durability of the coating, which promises great potential for applications in various touch screens, windows for hygiene environments, and optical apparatuses for medical uses such as endoscope, and so on.

  11. Designing novel hybrid materials by one-pot co-condensation: from hydrophobic mesoporous silica nanoparticles to superamphiphobic cotton textiles.

    Science.gov (United States)

    Pereira, C; Alves, C; Monteiro, A; Magén, C; Pereira, A M; Ibarra, A; Ibarra, M R; Tavares, P B; Araújo, J P; Blanco, G; Pintado, J M; Carvalho, A P; Pires, J; Pereira, M F R; Freire, C

    2011-07-01

    This work reports the synthesis and characterization of mesoporous silica nanoparticles (MSNs) functionalized with tridecafluorooctyltriethoxysilane (F13) and their in situ incorporation onto cotton textiles. The hybrid MSNs and the functional textiles were prepared by a one-pot co-condensation methodology between tetraethylorthosilicate (TEOS) and F13, with hexadecyltrimethylammonium chloride (CTAC) as the template and triethanolamine as the base. The influence of the F13 to TEOS molar ratio (1:10, 1:5 and 1:3) on the nanoparticle morphology, porosity, degree of functionalization, and hydro/oleophobic properties is discussed. The hybrid nanosilicas presented high colloidal stability and were spherical and monodispersed with average particle size of ∼45 nm. They also showed high surface areas, large pore volumes, and a wormhole-type mesoporous structure. The increase in the organosilane proportion during the co-condensation process led to a more radially branched wormhole-like mesoporosity, a decrease in the surface area, pore volume, and amount of surface silanol groups, and an enrichment of the surface with fluorocarbon moieties. These changes imparted hydrophobic and oleophobic properties to the materials, especially to that containing the highest F13 loading. Cotton textiles were coated with the F13-MSNs through an efficient and less time-consuming route. The combination between surface roughness and mesoporosity imparted by the MSNs, and the low surface energy provided by the organosilane resulted in superhydrophobic functional textiles. Moreover, the textile with the highest loading of fluorocarbon groups was superamphiphobic.

  12. One-pot template-free synthesis of monodisperse zinc sulfide hollow spheres and their photocatalytic properties.

    Science.gov (United States)

    Yu, Xiaoxiao; Yu, Jiaguo; Cheng, Bei; Huang, Baibiao

    2009-07-06

    Monodisperse wurtzite ZnS hollow spheres with diameters of about 200 nm and shells composed of nanoparticles have been successfully synthesized in high yield by a one-pot template-free hydrothermal route. The reaction duration, reactant species, and reaction temperature have been shown to play important roles in the formation of ZnS hollow spheres. X-ray diffraction, scanning and transmission electron microscopy, nitrogen adsorption/desorption, UV/Vis diffuse reflectance spectroscopy, and photoluminescence were used to characterize the products. The results show that all the prepared nanospheres have hexagonal wurtzite structures and exhibit good size uniformity and regularity. A mechanism for the formation of the ZnS hollow spherical structure by localized Ostwald ripening has been proposed based on experimental observations. In addition, studies of the photocatalytic properties of the ZnS hollow spheres by exposure to UV irradiation have demonstrated that they have potential photocatalytic applications. Hydroxyl radicals (*OH) were not detected on the surface of UV-illuminated ZnS by the photoluminescence technique, which suggests that *OH is not the dominant photo-oxidant and a photogenerated hole could instead directly participate in the photocatalytic reaction. The prepared ZnS hollow spheres are also of great interest for use in flat displays, sensors, lasers, catalysis, separation technology, biomedical engineering, and nanotechnology.

  13. Surface modification of magnesium aluminum hydroxide nanoparticles with poly(methyl methacrylate) via one-pot in situ polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Guo Xiaojun, E-mail: guoxj6906@163.com [College of Chemistry and Chemical Engineering, Northwest Normal University, 967 Anning East Road, Lanzhou 730070 (China); Zhao Leihua; Zhang Li; Li Jing [College of Chemistry and Chemical Engineering, Northwest Normal University, 967 Anning East Road, Lanzhou 730070 (China)

    2012-01-15

    Hydrophobic magnesium aluminum hydroxide composite particles (PMMA-MAH) were obtained by means of grafting poly(methyl methacrylate) (PMMA) onto the surface of magnesium aluminum hydroxide(MAH) nanoparticles after a novel type of phosphate coupling agent (DN-27) modification. The introduction of functional double bonds was firstly conducted on the surface of nanoparticles by DN-27 modification, followed by one-pot in situ polymerization on the particles surface using methyl methacrylate (MMA) as monomer, azoisobutyronitrile (AIBN) as initiator and sodium dodecyl sulfate (SDS) as stabilizer to graft PMMA on the surface of DN-27-modified MAH particles. The obtained composite particles were characterized by field-emission scanning electron microscope (FESEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray powder diffraction (XRD). The results show that the organic macromolecule PMMA could be successfully grafted on the surface of DN-27-modified MAH nanoparticles and the thermal stability of the PMMA-MAH composite particles had been improved. Compared with unmodified blank MAH sample, the product obtained with this method possesses better hydrophobic properties such as a higher water contact angle of 108 Degree-Sign and a well dispersion.

  14. Continuous, One-pot Synthesis and Post-Synthetic Modification of NanoMOFs Using Droplet Nanoreactors

    Science.gov (United States)

    Jambovane, Sachin R.; Nune, Satish K.; Kelly, Ryan T.; McGrail, B. Peter; Wang, Zheming; Nandasiri, Manjula I.; Katipamula, Shanta; Trader, Cameron; Schaef, Herbert T.

    2016-01-01

    Metal-organic frameworks (MOFs); also known as porous coordination polymers (PCP) are a class of porous crystalline materials constructed by connecting metal clusters via organic linkers. The possibility of functionalization leads to virtually infinite MOF designs using generic modular methods. Functionalized MOFs can exhibit interesting physical and chemical properties including accelerated adsorption kinetics and catalysis. Although there are discrete methods to synthesize well-defined nanoscale MOFs, rapid and flexible methods are not available for continuous, one-pot synthesis and post-synthetic modification (functionalization) of MOFs. Here, we show a continuous, scalable nanodroplet-based microfluidic route that not only facilitates the synthesis of MOFs at a nanoscale, but also offers flexibility for direct functionalization with desired functional groups (e.g., -COCH3, fluorescein isothiocyanate; FITC). In addition, the presented route of continuous manufacturing of functionalized nanosized MOFs takes significantly less time compared to state-of-the-art batch methods currently available (1 hr vs. several days). We envisage our approach to be a breakthrough method for synthesizing complex functionalized nanomaterials (metal, metal oxides, quantum dots and MOFs) that are not accessible by direct batch processing and expand the range of a new class of functionalized MOF-based functional nanomaterials. PMID:27821866

  15. Preparation of stable magnetic nanofluids containing Fe3O4@PPy nanoparticles by a novel one-pot route

    Directory of Open Access Journals (Sweden)

    Zhao Baobao

    2011-01-01

    Full Text Available Abstract Stable magnetic nanofluids containing Fe3O4@Polypyrrole (PPy nanoparticles (NPs were prepared by using a facile and novel method, in which one-pot route was used. FeCl3·6H2O was applied as the iron source, and the oxidizing agent to produce PPy. Trisodium citrate (Na3cit was used as the reducing reagent to form Fe3O4 NPs. The as-prepared nanofluid can keep long-term stability. The Fe3O4@PPy NPs can still keep dispersing well after the nanofluid has been standing for 1 month and no sedimentation is found. The polymerization reaction of the pyrrole monomers took place with Fe3+ ions as the initiator, in which these Fe3+ ions remained in the solution adsorbed on the surface of the Fe3O4 NPs. Thus, the core-shell NPs of Fe3O4@PPy were obtained. The particle size of the as-prepared Fe3O4@PPy can be easily controlled from 7 to 30 nm by the polymerization reaction of the pyrrole monomers. The steric stabilization and weight of the NPs affect the stability of the nanofluids. The as-prepared Fe3O4@PPy NPs exhibit superparamagnetic behavior.

  16. One-Pot Large-Scale Synthesis of Carbon Quantum Dots: Efficient Cathode Interlayers for Polymer Solar Cells.

    Science.gov (United States)

    Yang, Yuzhao; Lin, Xiaofeng; Li, Wenlang; Ou, Jiemei; Yuan, Zhongke; Xie, Fangyan; Hong, Wei; Yu, Dingshan; Ma, Yuguang; Chi, Zhenguo; Chen, Xudong

    2017-05-03

    Cathode interlayers (CILs) with low-cost, low-toxicity, and excellent cathode modification ability are necessary for the large-scale industrialization of polymer solar cells (PSCs). In this contribution, we demonstrated one-pot synthesized carbon quantum dots (C-dots) with high production to serve as efficient CIL for inverted PSCs. The C-dots were synthesized by a facile, economical microwave pyrolysis in a household microwave oven within 7 min. Ultraviolet photoelectron spectroscopy (UPS) studies showed that the C-dots possessed the ability to form a dipole at the interface, resulting in the decrease of the work function (WF) of cathode. External quantum efficiency (EQE) measurements and 2D excitation-emission topographical maps revealed that the C-dots down-shifted the high energy near-ultraviolet light to low energy visible light to generate more photocurrent. Remarkably improvement of power conversion efficiency (PCE) was attained by incorporation of C-dots as CIL. The PCE was boosted up from 4.14% to 8.13% with C-dots as CIL, which is one of the best efficiency for i-PSCs used carbon based materials as interlayers. These results demonstrated that C-dots can be a potential candidate for future low cost and large area PSCs producing.

  17. One-Pot Green Synthesis and Bioapplication ofl-Arginine-Capped Superparamagnetic Fe3O4 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Lai Yongchao

    2009-01-01

    Full Text Available Abstract Water-solublel-arginine-capped Fe3O4 nanoparticles were synthesized using a one-pot and green method. Nontoxic, renewable and inexpensive reagents including FeCl3,l-arginine, glycerol and water were chosen as raw materials. Fe3O4 nanoparticles show different dispersive states in acidic and alkaline solutions for the two distinct forms of surface bindingl-arginine. Powder X-ray diffraction and X-ray photoelectron spectroscopy were used to identify the structure of Fe3O4 nanocrystals. The products behave like superparamagnetism at room temperature with saturation magnetization of 49.9 emu g−1 and negligible remanence or coercivity. In the presence of 1-ethyl-3-(dimethylaminopropyl carbodiimide hydrochloride, the anti-chloramphenicol monoclonal antibodies were connected to thel-arginine-capped magnetite nanoparticles. The as-prepared conjugates could be used in immunomagnetic assay. (See supplementary material 1 Electronic supplementary material The online version of this article (doi:10.1007/s11671-009-9480-x contains supplementary material, which is available to authorized users. Click here for file

  18. Fabrication of γ-MnS/rGO composite by facile one-pot solvothermal approach for supercapacitor applications

    Science.gov (United States)

    Li, Xianfu; Shen, Jianfeng; Li, Na; Ye, Mingxin

    2015-05-01

    γ-MnS/reduced graphene oxide (γ-MnS/rGO) composite was successfully fabricated via a facile one-pot solvothermal route using graphene oxide (GO), thioacetamide (TAA, CH3CSNH2) and MnCl2·4H2O as reactants. It reveals that TAA plays an important role in reducing GO and sulfurizing γ-MnS. The synthesized composite was characterized via X-ray diffraction and scanning electron microscopy for structural and morphological studies. Electrochemical performance was also investigated through cyclic voltammetry and galvanostatic charge-discharge. As for the application of supercapacitors, the γ-MnS/rGO composite shows a great value of 802.5 F g-1 at a current density of 5 A g-1. Furthermore, the capacitance of γ-MnS/rGO has no decrease of its initial values after 2000 cycles. The galvanostatic charge-discharge curve demonstrates the ideal capacitive behavior of γ-MnS/rGO composite electrodes.

  19. One-Pot Synthesis of Graphene-Sulfur Composites for Li-S Batteries: Influence of Sulfur Precursors

    Directory of Open Access Journals (Sweden)

    James Guo Sheng Moo

    2017-12-01

    Full Text Available Lithium-sulfur (Li-S batteries are postulated as next-generation electrochemical energy storage devices due to their increased storage capabilities. However, challenges persist from the polysulfide-shuttle effect at the cathode. Soluble sulfur-based species in the cathode cross over to the lithium anode through the separator leading to fading capacity with cycling. This has spurred continuous effort by the scientific community to develop novel cathodes where sulfur species can affix better. A conductive nanostructured graphene network is a suitable candidate that can serve as a scaffold for holding sulfur nanoparticles. Here, a one-pot synthesis of chemically reduced graphene oxide networks prepared from easily accessible graphene oxide is demonstrated. The solution-based method simply allows for impregnation of the graphene oxide network with sulfur nanoparticles through a careful manipulation of pH of the chemical environment. Two routes were chosen for the precipitation of such sulfur nanoparticles: firstly, the dissolution of sulfur in sodium hydroxide into polysulfides followed by acidification and secondly, the acidification of sodium thiosulfate from alkaline media into sulfur nanoparticles. Both graphene oxide materials from the two routes were treated with sodium borohydride to achieve conductive graphene. The second route, with the sulfur nanoparticles derived from the acidification of sodium thiosulfate with chemically reduced graphene oxide, demonstrated favorable electrochemical behavior, showing promise as electrode material for Li-S batteries.

  20. Tuning of Activated Carbon for Solvent-Free Oxidation of Cyclohexane

    Directory of Open Access Journals (Sweden)

    Mohammad Sadiq

    2017-01-01

    Full Text Available Activated carbon (AC was prepared from carbonization of phosphoric acid soaked peanut shell at 380°C under inert atmosphere followed by activation with hydrogen peroxide. The AC was characterized by SEM, EDX, FTIR, TGA, and BET surface area and pore size analyzer. The potential of AC as a catalyst for solvent-free oxidation of cyclohexane to cyclohexanol and cyclohexanone (the mixture is known as KA oil in the presence of molecular oxygen at moderate temperature was investigated in a self-designed double-walled three-necked batch reactor. The effect of different reaction parameters/additive was optimized. The maximum productivity value (2.14 mmolg−1 h−1, without base, and 4.85 mmolg−1 h−1, with 0.2 mmol NaOH of the desired product was achieved under optimal reaction parameters: vol 12.5 mL, cat 0.4 g, time 14 h, oxygen flow 40 mL/min (pO2 760 Torr, stirring 1100 rpm, and temp 75°C. The AC shows recyclability for multiple runs without any significant loss in activity. Thus, the AC can be an efficient catalyst, due to low cost, ease of synthesis, easy recovery, nonleaching, and recyclability for multiple uses for the solvent-free oxidation of cyclohexane.

  1. Solvent-Free Synthesis of Flavour Esters through Immobilized Lipase Mediated Transesterification

    Directory of Open Access Journals (Sweden)

    Vijay Kumar Garlapati

    2013-01-01

    Full Text Available The synthesis of methyl butyrate and octyl acetate through immobilized Rhizopus oryzae NRRL 3562 lipase mediated transesterification was studied under solvent-free conditions. The effect of different transesterification variables, namely, molarity of alcohol, reaction time, temperature, agitation, addition of water, and enzyme amount on molar conversion (% was investigated. A maximum molar conversion of 70.42% and 92.35% was obtained in a reaction time of 14 and 12 h with the transesterification variables of 0.6 M methanol in vinyl butyrate and 2 M octanol in vinyl acetate using 80 U and 60 U immobilized lipase with the agitation speed of 200 rpm and 0.2% water addition at 32°C and 36°C for methyl butyrate and octyl acetate, respectively. The immobilized enzyme has retained good relative activity (more than 95% up to five and six recycles for methyl butyrate and octyl acetate, respectively. Hence, the present investigation makes a great impingement in natural flavour industry by introducing products synthesized under solvent-free conditions to the flavour market.

  2. Solvent-Free Synthesis of Flavour Esters through Immobilized Lipase Mediated Transesterification

    Science.gov (United States)

    Banerjee, Rintu

    2013-01-01

    The synthesis of methyl butyrate and octyl acetate through immobilized Rhizopus oryzae NRRL 3562 lipase mediated transesterification was studied under solvent-free conditions. The effect of different transesterification variables, namely, molarity of alcohol, reaction time, temperature, agitation, addition of water, and enzyme amount on molar conversion (%) was investigated. A maximum molar conversion of 70.42% and 92.35% was obtained in a reaction time of 14 and 12 h with the transesterification variables of 0.6 M methanol in vinyl butyrate and 2 M octanol in vinyl acetate using 80 U and 60 U immobilized lipase with the agitation speed of 200 rpm and 0.2% water addition at 32°C and 36°C for methyl butyrate and octyl acetate, respectively. The immobilized enzyme has retained good relative activity (more than 95%) up to five and six recycles for methyl butyrate and octyl acetate, respectively. Hence, the present investigation makes a great impingement in natural flavour industry by introducing products synthesized under solvent-free conditions to the flavour market. PMID:23819043

  3. Lipase Mediated Isoamyl Acetate Synthesis in Solvent-Free System Using Vinyl Acetate as Acyl Donor

    Directory of Open Access Journals (Sweden)

    Annapurna Kumari

    2009-01-01

    Full Text Available Synthesis of isoamyl acetate, a flavour ester extensively used in food industry, has been carried out in a solvent-free system. In the present study, an attempt has been made to enhance the isoamyl acetate synthesis yield by transesterification of isoamyl alcohol with vinyl acetate using immobilized Rhizopus oryzae NRRL 3562 lipase. In the present synthesis, substrates had no inhibitory effect on immobilized lipase. The effects of various reaction parameters on isoamyl acetate synthesis were studied and maximum conversion was achieved at 16 % (by mass per volume of immobilized lipase, 40 °C and 200 rpm. Under these conditions, 8-hour reaction time was sufficient to reach a high ester conversion of 95 % with 0.5 mol/L of isoamyl alcohol. The structure of the transesterified product was confirmed by infrared and nuclear magnetic resonance spectroscopic studies. Immobilized lipase had Km and vmax values of 306.53 mmol/L and 99 µmol/(h·g respectively, for isoamyl acetate synthesis in a solvent-free system.

  4. Durability of solvent-free one-step self-etch adhesive under simulated intrapulpal pressure.

    Science.gov (United States)

    Nagi, Shaymaa M

    2015-10-01

    There are different solvents presented in simplified adhesives. Bond-1 SF has been developed, which contains neither water nor organic solvents, in order to eliminate technical issues in terms of evaporation of solvents and concerns for the durability of resin-dentin bond. Thus this study was conducted to evaluate the microtensile bond strength (?TBS) of solvent-free and ethanol-based one-step self-etch adhesives to dentin under simulated intrapulpal pressure (IPP). Occlusal surfaces of human molars were prepared to expose mid-dentin depth. Bond-1SF Solvent-Free SE [SF] and AdperTM easy one adhesives [AE] were applied on dentin specimens. Resin composite build up was done in increments. Then specimens were stored under simulated IPP 20 mmHg, immersed in artificial saliva at 37 ºC for 24 hours (24h) and 6 months (6m). Specimens were sectioned into sticks of (1 mm²) to be tested for (?TBS) using a universal testing machine. Both fractured sections of each stick were inspected using a stereomicroscope at 40× magnification to determine the mode of failure. Data were statistically analyzed by Two-way ANOVA of Variance. There was no statistically significant difference between the mean ?TBS of both [SF] and [AE] adhesives at both aging periods, 24h and 6m (pself-etch adhesives, solvents.

  5. Ultra-high dispersion of graphene in polymer composite via solvent free fabrication and functionalization

    Science.gov (United States)

    Noh, Ye Ji; Joh, Han-Ik; Yu, Jaesang; Hwang, Soon Hyoun; Lee, Sungho; Lee, Cheol Ho; Kim, Seong Yun; Youn, Jae Ryoun

    2015-03-01

    The drying process of graphene-polymer composites fabricated by solution-processing for excellent dispersion is time consuming and suffers from a restacking problem. Here, we have developed an innovative method to fabricate polymer composites with well dispersed graphene particles in the matrix resin by using solvent free powder mixing and in-situ polymerization of a low viscosity oligomer resin. We also prepared composites filled with up to 20 wt% of graphene particles by the solvent free process while maintaining a high degree of dispersion. The electrical conductivity of the composite, one of the most significant properties affected by the dispersion, was consistent with the theoretically obtained effective electrical conductivity based on the mean field micromechanical analysis with the Mori-Tanaka model assuming ideal dispersion. It can be confirmed by looking at the statistical results of the filler-to-filler distance obtained from the digital processing of the fracture surface images that the various oxygenated functional groups of graphene oxide can help improve the dispersion of the filler and that the introduction of large phenyl groups to the graphene basal plane has a positive effect on the dispersion.

  6. A general three-step one-pot synthesis of novel (E)-6-chloro-2-(aryl/hetarylvinyl)quinoline-3-carboxylic acids.

    Science.gov (United States)

    Li, Yang; Wang, Yang; Zou, Hongtao

    2017-05-01

    In this work, a facile and general three-step one-pot synthesis of structurally new (E)-6-chloro-2-(aryl/hetarylvinyl)quinoline-3-carboxylic acid derivatives has been achieved from easily available ethyl 6-chloro-2-(chloromethyl) quinoline-3-carboxylate and aromatic or heteroaromatic aldehydes. This strategy features simple one-pot operation, tolerance of a wide range of substituents, and good yields. Moreover, these newly synthesized compounds belong to a new class of quinoline derivatives and could be good candidates for the development of more complex quinoline compounds for use in medicinal chemistry.

  7. EFFICIENT SODIUM SELENATE-CATALYZED SYNTHESIS OF 3,4 ...

    African Journals Online (AJOL)

    Sodium selenate efficiently catalyzes the three-component Biginelli reaction of an aldehyde, a,β-keto ester and urea or thiourea under solvent-free conditions to afford the corresponding 3,4-dihydropyrimidin-2(1H)-ones or –thiones in excellent yields. KEY WORDS: Dihydropyrimidinones, Sodium selenate, Biginelli reaction, ...

  8. Supporting Information TMSCl-catalyzed condensation of α-diketone ...

    Indian Academy of Sciences (India)

    Administrator

    Supporting Information. TMSCl-catalyzed condensation of α-diketone compounds with urea/thiourea derivatives under solvent-free conditions. Akbar Mobinikhaledi* and Alireza Khajeh Amiri. Department of Chemistry, Faculty of Science, Arak University, Tel: +98 861 4173415,. P.O. Box 14335-186, Arak, Iran. Fax: +98 861 ...

  9. One-pot solvothermal synthesis of highly water-dispersible size-tunable functionalized magnetite nanocrystal clusters for lipase immobilization.

    Science.gov (United States)

    Zhu, Hao; Hou, Chen; Li, Yijing; Zhao, Guanghui; Liu, Xiao; Hou, Ke; Li, Yanfeng

    2013-07-01

    A facile one-pot synthesis of highly water-dispersible size-tunable magnetite (Fe3O4) nanocrystal clusters (MNCs) end-functionalized with amino or carboxyl groups by a modified solvothermal reduction reaction has been developed. Dopamine and 3,4-dihydroxyhydroxycinnamic acid were used for the first time as both a surfactant and interparticle linker in a polylol process for economical and environment-friendly purposes. Morphology, chemical composition, and magnetic properties of the prepared particles were investigated by several methods, including FESEM, TEM, XRD, XPS, Raman, FTIR, TGA, zeta potential, and VSM. The sizes of the particles could be easily tuned over a wide range from 175 to 500 nm by varying the surfactant concentration. Moreover, ethylene glycol/diethylene glycol (EG/DEG) solvent mixtures with different ratios could be used as reductants to obtain the particles with smaller sizes. The XRD data demonstrated that the surfactants restrained the crystal growth of the grains. The nanoparticles showed superior magnetic properties and high colloidal stability in water. The cytotoxicity results indicated the feasibility of using the synthesized nanocrystals in biology-related fields. To estimate the applicability of the obtained MNCs in biotechnology, Candida rugosa lipase was selected for the enzyme immobilization process. The immobilized lipase exhibited excellent thermal stability and reusability in comparison with the free enzyme. This novel strategy would simplify the reaction protocol and improve the efficiency of materials functionalization, thus offering new potential applications in biotechnology and organocatalysis. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Microwave-assisted one-pot synthesis of metal/metal oxide nanoparticles on graphene and their electrochemical applications

    International Nuclear Information System (INIS)

    Wang Shuangyin; Jiang San Ping; Wang Xin

    2011-01-01

    Graphical abstract: Display Omitted Research highlights: → Microwave polyol method is efficient to deposit nanoparticles on graphene. → SnO 2 /graphene is more efficient than graphene for supercapacitor. → PtRu/graphene is more active than commercial PtRu/C for methanol oxidation. - Abstract: An effective synthesis strategy of hybrid metal (PtRu)/metal oxide (SnO 2 ) nanoparticles on graphene nanocomposites is developed using a microwave-assisted one-pot reaction process. The mixture of ethylene glycol (EG) and water is used as both solvent and reactant. In the reaction system for the synthesis of SnO 2 /graphene nanocomposite, EG not only reduces graphene oxide (GO) to graphene, but also results in the formation of SnO 2 facilitated by the presence of a small amount of water. On the other hand, in the reaction system for preparation of PtRu/graphene nanocomposites, EG acts as solvent and reducing agent for reduction of PtRu nanoparticles from their precursors and reduction of graphene from graphene oxide. Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) characterizations confirm the feasibility of the microwave-assisted reaction system to simultaneously reduce graphene oxide and to form SnO 2 or PtRu nanoparticles. The as-synthesized SnO 2 /graphene hybrid composites show a much higher supercapacitance than the pure graphene, and the as-prepared PtRu/graphene show much better electrocatalytic activity for methanol oxidation compared to the commercial E-TEK PtRu/C electrocatalysts.

  11. One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

    International Nuclear Information System (INIS)

    Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin; Ho, Jeffery Weng Chye; Tay, Yee Yan; Lau, Wei Siew; Wijaya, Olivia; Lim, Jiexiang; Chen, Zhong

    2014-01-01

    Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO 2 . The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB

  12. One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Yu Hua; Gong, Dangguo; Tang, Yuxin; Ho, Jeffery Weng Chye; Tay, Yee Yan; Lau, Wei Siew; Wijaya, Olivia; Lim, Jiexiang; Chen, Zhong, E-mail: aszchen@ntu.edu.sg

    2014-06-01

    Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO{sub 2}. The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB.

  13. A catechol-like phenolic ligand-functionalized hydrothermal carbon: One-pot synthesis, characterization and sorption behavior toward uranium

    Energy Technology Data Exchange (ETDEWEB)

    Li, Bo; Ma, Lijian; Tian, Yin; Yang, Xiaodan; Li, Juan; Bai, Chiyao; Yang, Xiaoyu; Zhang, Shuang; Li, Shoujian, E-mail: sjli000616@scu.edu.cn; Jin, Yongdong, E-mail: jinyongdong@scu.edu.cn

    2014-04-01

    Highlights: • A new catechol-like ligand-functionalized hydrothermal carbon sorbent is synthesized. • A combination of bayberry tannin and glyoxal is firstly used as starting materials. • Simple, economically viable and environment-friendly synthesis method. • The sorbent exhibits high sorption capacity and distinct selectivity for uranium. - Abstract: We proposed a new approach for preparing an efficient uranium-selective solid phase extractant (HTC-btg) by choosing bayberry tannin as the main building block and especially glyoxal as crosslinking agent via a simple, economic, and green one-pot hydrothermal synthesis. The results of characterization and analysis show that after addition of glyoxal into only bayberry tannin-based hydrothermal reaction system, the as-synthesized HTC-btg displayed higher thermal stability, larger specific surface area and more than doubled surface phenolic hydroxyl groups. The sorption behavior of the sorbents toward uranium under various conditions was investigated in detail and the results indicated that the process is fast, endothermic, spontaneous, and pseudo-second-order chemisorption. The U(VI) sorption capacity reached up to 307.3 mg g{sup −1} under the current experimental conditions. The selective sorption in a specially designed multi-ion solution containing 12 co-existing cations over the range of pH 1.0–4.5 shown that the amount of uranium sorbed accounts for about 53% of the total sorption amount at pH 4.5 and distinctively about 85%, unreported so far to our knowledge, at pH 2.0. Finally, a possible mechanism involving interaction between uranyl ions and phenolic hydroxyl groups on HTC-btg was proposed.

  14. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Nali [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Ren, Yapeng; Kong, Peipei; Tan, Lin [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Feng, Huixia, E-mail: fenghx@lut.cn [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Luo, Yongchun, E-mail: luoyc@lut.cn [State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China)

    2017-01-15

    Highlights: • A new method to prepare reduced graphene oxide/polyaniline composite is developed. • Aniline serves as a reduction for graphene oxide under weak alkali condition. • Different characterizations confirm that GO can be effectively reduced by aniline. • A high specific capacitance of 524.4 F·g{sup −1} is obtained at 0.5 A·g{sup −1}. - Abstract: Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  15. Antimicrobial nanocapsules: from new solvent-free process to in vitro efficiency

    Directory of Open Access Journals (Sweden)

    Steelandt J

    2014-09-01

    Full Text Available Julie Steelandt,1 Damien Salmon,1,2 Elodie Gilbert,1 Eyad Almouazen,3 François NR Renaud,4 Laurène Roussel,1 Marek Haftek,5 Fabrice Pirot1,2 1University Claude Bernard Lyon 1, Faculty of Pharmacy, Fundamental, Clinical and Therapeutic Aspects of Skin Barrier Function, FRIPharm, Laboratoire de Pharmacie Galénique Industrielle, 2Hospital Pharmacy, FRIPharm, Hospital Edouard Herriot, Hospices Civils de Lyon, 3Laboratoire d’Automatique et de Génie des Procédés, University Claude Bernard Lyon 1, 4University Claude Bernard Lyon 1, UMR CNRS 5510/MATEIS, 5University Claude Bernard Lyon 1, Faculty of Pharmacy, Fundamental, Clinical and Therapeutic Aspects of Skin Barrier Function, FRIPharm, Laboratoire de Dermatologie, Lyon, France Abstract: Skin and mucosal infections constitute recurrent pathologies resulting from either inappropriate antiseptic procedures or a lack of efficacy of antimicrobial products. In this field, nanomaterials offer interesting antimicrobial properties (eg, long-lasting activity; intracellular and tissular penetration as compared to conventional products. The aim of this work was to produce, by a new solvent-free process, a stable and easily freeze-dryable chlorhexidine-loaded polymeric nanocapsule (CHX-NC suspension, and then to assess the antimicrobial properties of nanomaterials. The relevance of the process and the physicochemical properties of the CHX-NCs were examined by the assessment of encapsulation efficiency, stability of the nanomaterial suspension after 1 month of storage, and by analysis of granulometry and surface electric charge of nanocapsules. In vitro antimicrobial activities of the CHX-NCs and chlorhexidine digluconate solution were compared by measuring the inhibition diameters of two bacterial strains (Escherichia coli and Staphylococcus aureus and one fungal strain (Candida albicans cultured onto appropriate media. Based on the findings of this study, we report a new solvent-free process for the

  16. Solvent-Free Selective Oxidation of Toluene with O2 Catalyzed by Metal Cation Modified LDHs and Mixed Oxides

    Directory of Open Access Journals (Sweden)

    Xiaoli Wang

    2016-01-01

    Full Text Available A series of metal cation modified layered-double hydroxides (LDHs and mixed oxides were prepared and used to be the selective oxidation of toluene with O2. The results revealed that the modified LDHs exhibited much higher catalytic performance than their parent LDH and the modified mixed oxides. Moreover, the metal cations were also found to play important roles in the catalytic performance and stabilities of modified catalysts. Under the optimal reaction conditions, the highest toluene conversion reached 8.7% with 97.5% of the selectivity to benzyldehyde; moreover, the catalytic performance remained after nine catalytic runs. In addition, the reaction probably involved a free-radical mechanism.

  17. A general and efficient synthesis of pyrazoles catalyzed by Sc(OTf)3 under solvent-free conditions

    OpenAIRE

    Xiong, Wei; Chen, Jiu-Xi; Liu, Miao-Chang; Ding, Jin-Chang; Wu, Hua-Yue; Su, Wei-Ke

    2009-01-01

    Pyrazoles were prepared in excellent yields via solventless condensation of various 1,3-diketones (R¹COCHXCOCH3, R¹ = Me, Ph; X = H, Me, Cl) and hydrazines, acylhydrazines or sulfonyl hydrazines in the presence of a catalytic amount of Sc(OTf)3 at room temperature. Additionally, the catalyst could be recovered easily after the reactions and reused without evident loss in activity. Pirazóis foram preparados em excelentes rendimentos via reação de condensação entre várias 1,3-dicetonas (R¹CO...

  18. {omicron}-iodoxybenzoic acid in water: optimized green alternative for multicomponent one-pot synthesis of 2-amino-3,5-dicarbonitrile-6-thiopyridines

    Energy Technology Data Exchange (ETDEWEB)

    Takale, Santosh; Patil, Jaidas; Pisal, Rajaram, E-mail: achaskar25@gmail.com [Changu Kana Thakur Research Centre, Mumbai (India); Padalkar, Vikas [Institute of Chemical Technology, Matunga, Mumbai (India); Chaskar, Atul [Department of Chemistry, National Taiwan University, Taipei (China)

    2012-05-15

    A multicomponent one-pot reaction of aromatic aldehyde, malononitrile and thiophenol in the presence of iodoxybenzoic acid (IBX) in aqueous media furnished 2-amino-3,5-dicarbonitrile- 6-thiopyridine in good to excellent yield. Eventually, a catalyst could be easily recovered and reused without loss of its catalytic property. (author)

  19. One-pot combination of enzyme and Pd nanoparticle catalysis for the synthesis of enantiomerically pure 1,2-amino alcohols

    NARCIS (Netherlands)

    Schrittwieser, J.; Coccia, F.; Kara, S.; Grischek, B.; Kroutil, W.; d'Alessandro, N.; Hollmann, F.

    2013-01-01

    One-pot combinations of sequential catalytic reactions can offer practical and ecological advantages over classical multi-step synthesis schemes. In this context, the integration of enzymatic and chemo-catalytic transformations holds particular potential for efficient and selective reaction

  20. One-pot Microwave-Assisted Synthesis of 1H-Phenanthro[9,10- d][1,2,3]triazole

    Directory of Open Access Journals (Sweden)

    Mehrak Faraji

    2008-09-01

    Full Text Available In this study, a fast and good yield one-pot microwave-assisted synthesis (45 seconds of 1H-phenanthro[9,10-d][1,2,3]triazole by a 1,3-dipolar cycloaddition reaction of sodium azide and 9-bromophenanthrene in the presence of potassium tert-butoxide in DMSO as solvent is reported.

  1. Synthesis of unnatural amino acids via microwave-assisted regio-selective one-pot multi-component reactions of sulfamidates

    Science.gov (United States)

    Synthesis of triazole-based unnatural amino acids, triazole bisaminoacids and β-amino triazole has been described via stereo and regioselective one-pot multi-component reaction of sulfamidates, sodium azide, and alkynes under MW irradiation conditions. The developed method is app...

  2. Instantaneous one-pot synthesis of Fe-N-modified graphene as an efficient electrocatalyst for the oxygen reduction reaction in acidic solutions.

    Science.gov (United States)

    Kamiya, Kazuhide; Hashimoto, Kazuhito; Nakanishi, Shuji

    2012-10-21

    We successfully developed a one-pot synthesis method of graphenes modified with iron and nitrogen. The modified graphenes functioned as an efficient electrocatalyst for the oxygen reduction reaction in acidic solutions with an onset-potential of 850 mV vs. RHE in acidic solutions.

  3. A Convenient One-Pot Preparation of 2-Methyl-3-(phenylthio- methylquinolines from Morita-Baylis-Hillman Adducts and Their Oxidation to the Corresponding Sulfones

    Directory of Open Access Journals (Sweden)

    Ching-Fa Yao

    2012-05-01

    Full Text Available A convenient one-pot preparation of 2-methyl-3-(phenylthiomethylquinolines from Morita-Baylis-Hillman adducts via conjugate addition of thiols followed by reductive cyclization with Fe/AcOH was developed. The 2-methyl-3-(phenylthiomethylquinolines were transformed into 2-methyl-3-(phenylsulfonylmethylquinolines via m-CPBA-mediated oxidation.

  4. Facile one-pot synthesis of spherical zinc sulfide-carbon nanocomposite powders with superior electrochemical properties as anode materials for Li-ion batteries.

    Science.gov (United States)

    Jang, Yong Seung; Kang, Yun Chan

    2013-10-21

    A novel and simple one-pot method of systematically synthesizing spherical metal sulfide-carbon composite powders is reported for the first time. The zinc sulfide-carbon composite is selected as the first target material. The prepared composite powders show superior electrochemical properties as anode materials for lithium-ion batteries.

  5. A one-pot synthesis of 1,6,9,13-tetraoxadispiro(4.2.4.2)tetradecane by hydrodeoxygenation of xylose using a palladium catalyst

    Science.gov (United States)

    In an effort to expand the number of biobased chemicals available from sugars, xylose has been converted to 1,6,9,13-tetraoxadispiro(4.2.4.2)tetradecane in a one-pot reaction using palladium supported on silica-alumina as the catalyst. The title compound is produced in 35-40% yield under 7 MPa H2 pr...

  6. A Robust, "One-Pot" Method for Acquiring Kinetic Data for Hammett Plots Used to Demonstrate Transmission of Substituent Effects in Reactions of Aromatic Ethyl Esters

    Science.gov (United States)

    Yau, Hon Man; Haines, Ronald S.; Harper, Jason B.

    2015-01-01

    A "one-pot" method for acquiring kinetic data for the reactions of a series of substituted aromatic esters with potassium hydroxide using [supserscript 13]C NMR spectroscopy is described, which provides an efficient way to obtain sufficient data to demonstrate the Hammett equation in undergraduate laboratories. The method is…

  7. A One-Pot Selective Synthesis of N-Boc Protected Secondary Amines: Tandem Direct Reductive Amination/N-Boc Protection

    OpenAIRE

    Neelarapu, Raghupathi; Petukhov, Pavel A.

    2012-01-01

    A one-pot tandem direct reductive amination of aldehydes with primary amines resulting in N-Boc secondary amines using a (Boc)2O/sodium triacetoxyborohydride (STAB) system is reported. The tandem procedure is efficient, selective, and versatile, giving excellent yields of N-Boc protected secondary amines even in those cases where the products are prone to intramolecular lactamization

  8. A One-Pot Selective Synthesis of N-Boc Protected Secondary Amines: Tandem Direct Reductive Amination/N-Boc Protection.

    Science.gov (United States)

    Neelarapu, Raghupathi; Petukhov, Pavel A

    2012-09-02

    A one-pot tandem direct reductive amination of aldehydes with primary amines resulting in N-Boc secondary amines using a (Boc)(2)O/sodium triacetoxyborohydride (STAB) system is reported. The tandem procedure is efficient, selective, and versatile, giving excellent yields of N-Boc protected secondary amines even in those cases where the products are prone to intramolecular lactamization.

  9. Solvent free microwave assisted preparation of new telechelic polymers based on poly(ethylene glycol

    Directory of Open Access Journals (Sweden)

    2009-07-01

    Full Text Available Poly(ethylene glycol bis (methylimidazolium chloride (PEGBMIM with average molecular weights of 600 and 1000 g/mol and poly(ethylene glycol bis (2-oxazoline (PEGBOX with average molecular weight of 600 g/mol have been prepared using microwave irradiation under solvent-free condition. The method described herein is a very good, safe, clean, economical and environmentally friendly alternative to the classical procedures. The resulted products have been characterized by common spectroscopic methods, such as FT-IR (Fourier transform infrared spectroscopy, 1H NMR (Nuclear magnetic resonance of proton and elemental analysis. Also, the effects of power levels and irradiation time on the yield of reactions and solubility of products have been studied.

  10. Structure of solvent-free grafted nanoparticles: Molecular dynamics and density-functional theory

    KAUST Repository

    Chremos, Alexandros

    2011-01-01

    The structure of solvent-free oligomer-grafted nanoparticles has been investigated using molecular dynamics simulations and density-functional theory. At low temperatures and moderate to high oligomer lengths, the qualitative features of the core particle pair probability, structure factor, and the oligomer brush configuration obtained from the simulations can be explained by a density-functional theory that incorporates the configurational entropy of the space-filling oligomers. In particular, the structure factor at small wave numbers attains a value much smaller than the corresponding hard-sphere suspension, the first peak of the pair distribution function is enhanced due to entropic attractions among the particles, and the oligomer brush expands with decreasing particle volume fraction to fill the interstitial space. At higher temperatures, the simulations reveal effects that differ from the theory and are likely caused by steric repulsions of the expanded corona chains. © 2011 American Institute of Physics.

  11. Solvent-free optical resolution of N-methylamphetamine by distillation after partial diastereoisomeric salt formation.

    Science.gov (United States)

    Kozma, D; Fogassy, E

    2001-08-01

    Solvent-free optical resolution of N-methylamphetamine was developed by distillation after partial diastereoisomeric salt formation. From the 18 chiral acids tested by this method, five provide by this method resolution: O,O'-dibenzoyltartaric acid, O,O'-di-p-toluoyltartaric acid, 6-methoxy-alpha-methyl-2-naphthaleneacetic acid (Naproxen), the cis-permetrinic acid, and the 2-phenoxypropionic acid. Among them the O,O'-dibenzoyltartaric acid in water-free form provided the more effective resolution. The efficiency of this resolution S = 0.74 is in the range of the industrial-scale resolutions and not worse than the efficiency achieved by optical resolution via fractional crystallization. Copyright 2001 Wiley-Liss, Inc.

  12. Solvent-Free Patterning of Colloidal Quantum Dot Films Utilizing Shape Memory Polymers

    Directory of Open Access Journals (Sweden)

    Hohyun Keum

    2017-01-01

    Full Text Available Colloidal quantum dots (QDs with properties that can be tuned by size, shape, and composition are promising for the next generation of photonic and electronic devices. However, utilization of these materials in such devices is hindered by the limited compatibility of established semiconductor processing techniques. In this context, patterning of QD films formed from colloidal solutions is a critical challenge and alternative methods are currently being developed for the broader adoption of colloidal QDs in functional devices. Here, we present a solvent-free approach to patterning QD films by utilizing a shape memory polymer (SMP. The high pull-off force of the SMP below glass transition temperature (Tg in conjunction with the conformal contact at elevated temperatures (above Tg enables large-area, rate-independent, fine patterning while preserving desired properties of QDs.

  13. Solvent-free synthesis of three layered manganese sulfate-oxalates with different pore apertures

    Science.gov (United States)

    Shi, Jingyu; Guo, Furong; Yang, Meng; Zeng, Hongmei; Lin, Zhien

    2018-01-01

    Three manganese sulfate-oxalates, namely, H2pip·Mn2(SO4)2(ox)(H2O)2·2H2O (1), H3ipaṡMn2(SO4)(ox)2.5·H2O (2), and H3dptaṡMn2(SO4)2(ox)1.5(H2O)3 (3), were prepared under solvent-free conditions, where pip = piperazine, ox = oxalate, ipa = 3,3‧-iminobis(N,N-dimethylpropylamine), and dpta = dipropylenetriamine. These compounds have different layered structures intercalated with organic cations. Their pore apertures range from small 8-membered ring (8 MR) to large 12 MR and extra-large 20 MR. The temperature dependence of the magnetic susceptibility of these compounds were also investigated.

  14. Development of a new solvent-free flow efficiency coating for natural gas pipelines

    Energy Technology Data Exchange (ETDEWEB)

    Fogg, Graham A.; Morse, Jennifer [Bredero Shaw, Houston, TX (United States)

    2005-07-01

    Pipeline design engineers have traditionally considered external anti-corrosion coatings for the protection of gas transmission pipelines, with less consideration given to the benefits of internal flow efficiency coatings. This paper reviews the benefits of using a traditional solvent-based flow efficiency coating, and the relationship between the internal surface roughness of a pipe, the pressure drop across the pipeline, and the maximum flow rate of gas through the pipeline. To improve upon existing solvent-based flow efficiency coatings, a research program was undertaken to develop a solvent-free coating. The stages in the development of this coating are discussed, resulting in the plant application of the coating and final qualification to API RP 5L2. (author)

  15. Microwave Synthesis Under Solvent-Free Conditions and Spectral Studies of Some Mesoporphyrinic Complexes

    Directory of Open Access Journals (Sweden)

    Rica Boscencu

    2012-05-01

    Full Text Available A series of A3B and A4 type mesoporphyrinic complexes were synthesized with superior yields using microwave irradiation under solvent-free conditions. The structures of the complexes were confirmed using elemental analysis, FT-IR, UV-Vis, EPR and NMR spectral data. The influence of environmental polarity on spectral properties of the mesoporphyrinic complexes was investigated. The obtained results indicate that the shape of absorption and fluorescence spectra does not depend on the solvent polarity under the experimental conditions used. The small shifts of the absorption and emission maximums that occur by increasing of solvent polarity reflects the physical interaction between the porphyrinic substituents and the solvent molecules.

  16. Solvent free low-melt viscosity imide oligomers and thermosetting polymide composites

    Science.gov (United States)

    Chuang, Chun-Hua (Inventor)

    2012-01-01

    .[.This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280.degree. C. When the imide oligomer melt is cured at about 371.degree. C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T.sub.g) equal to and above 310.degree. C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280.degree. C. (450-535.degree. F.) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343.degree. C. (550-650.degree. F.) high temperature performance capability..]. .Iadd.This invention relates to compositions and a solvent-free reaction process for preparing imide oligomers and polymers specifically derived from effective amounts of dianhydrides such as 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA), at least one aromatic polyamine and an end-cap such as 4-phenylethynyphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260.degree. C.-280.degree. C..Iaddend.

  17. Convenient synthesis of non-conjugated alkynyl ketones from keto aldehydes by a chemoselective one-pot nonaflation-base catalyzed elimination sequence

    Czech Academy of Sciences Publication Activity Database

    Boltukhina, Ekaterina; Sheshenev, Andrey; Lyapkalo, Ilya

    2011-01-01

    Roč. 67, č. 30 (2011), s. 5382-5388 ISSN 0040-4020 Institutional research plan: CEZ:AV0Z40550506 Keywords : nonaflation * alkynyl ketones * cross-coupling * elimination * phosphazene base Subject RIV: CC - Organic Chemistry Impact factor: 3.025, year: 2011

  18. One-pot, four-component synthesis of pyrano[2,3-c]pyrazoles catalyzed by sodium benzoate in aqueous medium

    Directory of Open Access Journals (Sweden)

    Hamzeh Kiyani

    2013-10-01

    Full Text Available An efficient, green, and facile four-component reaction for the preparation of pyrano[2,3-c]pyrazole derivatives through the condensation reaction of aryl aldehydes, ethyl acetoacetate, malononitrile, and hydrazine hydrate or phenyl hydrazine in the presence of commercially available organocatalyst sodium benzoate under aqueous condition is reported. The products are produced with high yields and in shorter reaction times. It also is mild, safe, green and environmental friendly.

  19. Iodine catalyzed one-pot synthesis of chloro-substituted linear and angular indoloquinolines and in vitro antiproliferative activity study of different indoloquinolines

    Digital Repository Service at National Institute of Oceanography (India)

    Parvatkar, P.T.; Ajay, A.K.; Bhat, M.K.; Parameswaran, P.S.; Tilve, S.G.

    -substituted 6H-indolo[2,3-b]quinoline 3c to be the most active and the parent 6H-indolo[2,3-b]quinoline 3a to be the least active, while the other compounds including the different chloro derivatives exhibited only intermediate activity....

  20. In situ one-pot preparation of superparamagnetic hydrophilic porous microspheres for covalently immobilizing penicillin G acylase to synthesize amoxicillin

    Science.gov (United States)

    Xue, Ping; Gu, Yaohua; Su, Weiguang; Shuai, Huihui; Wang, Julan

    2016-01-01

    Magnetic hydrophilic porous microspheres were successfully one-pot synthesized for the first time via in situ inverse suspension polymerization of glycidyl methacrylate, N,N‧-methylene bisacrylamide and 2-hydroxyethyl methacrylate in the presence of Fe3+ and Fe2+ dispersed in formamide, which were denoted as magnetic Fe3O4-GMH microspheres. The morphology and properties of magnetic Fe3O4-GMH microspheres were characterized by SEM, VSM, XRD, FTIR, and so on. The formamide content had an important influence on the morphology of Fe3O4-GMH, and nearly perfectly spherical Fe3O4-GMH particles were formed when the amount of formamide was 15 ml. The diameters of the microspheres were in the range of 100-200 μm and Fe3O4-GMH exhibited superparamagnetic behavior with the saturation magnetization of 5.44 emu/g. The specific surface area of microspheres was 138.7 m2/g, the average pore diameter and pore volume were 15.1 nm and 0.60 cm3/g, respectively. The content of oxirane groups on Fe3O4-GMH was 0.40 mmol/g. After penicillin G acylase (PGA) was covalently immobilized on Fe3O4-GMH microspheres, the catalytic performance for amoxicillin synthesis by 6-aminopenicillanic acid and D-hydroxyphenylglycine methyl ester was largely improved. As a result, 90.1% amoxicillin yield and 1.18 of the synthesis/hydrolysis (S/H) ratio were achieved on PGA/Fe3O4-GMH with ethylene glycol as solvent, but only 62.6% amoxicillin yield and 0.37 of the S/H ratio were obtained on free PGA under the same reaction conditions. Furthermore, the amoxicillin yield and S/H ratio were still kept at 88.2% and 1.06, respectively after the immobilized PGA was magnetically separated and recycled for 10 times, indicating that PGA/Fe3O4-GMH had a very good reusability.

  1. Comparison of microwave hydrodistillation and solvent-free microwave extraction of essential oil from Melaleuca leucadendra Linn

    Science.gov (United States)

    Ismanto, A. W.; Kusuma, H. S.; Mahfud, M.

    2017-12-01

    The comparison of solvent-free microwave extraction (SFME) and microwave hydrodistillation (MHD) in the extraction of essential oil from Melaleuca leucadendra Linn. was examined. Dry cajuput leaves were used in this study. The purpose of this study is also to determine optimal condition (microwave power). The relative electric consumption of SFME and MHD methods are both showing 0,1627 kWh/g and 0,3279 kWh/g. The results showed that solvent-free microwave extraction methods able to reduce energy consumption and can be regarded as a green technique for extraction of cajuput oil.

  2. Solvent-free, catalyst-free aza-Michael addition of cyclohexylamine to diethyl maleate: reaction mechanism and kinetics

    Czech Academy of Sciences Publication Activity Database

    Bláha, Michal; Trhlíková, Olga; Podešva, Jiří; Abbrent, Sabina; Steinhart, Miloš; Dybal, Jiří; Dušková-Smrčková, Miroslava

    2018-01-01

    Roč. 74, č. 1 (2018), s. 58-67 ISSN 0040-4020 Institutional support: RVO:61389013 Keywords : Aza-Michael addition * solvent-free * catalyst-free Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 2.651, year: 2016

  3. Noticeable facilitation of the bismuth-mediated Barbier-type allylation of aromatic carbonyl compounds under solvent-free conditions.

    Science.gov (United States)

    Wada, Shinobu; Hayashi, Nobuyuki; Suzuki, Hitomi

    2003-06-21

    When milled together with bismuth shot in the presence of allyl halide, aromatic aldehydes readily underwent a Barbier-type allylation to afford the corresponding homoallyl alcohols in good yield. In contrast to the failure in solution reaction, aromatic ketones also underwent allylic carbonyl addition under solvent-free conditions to give the expected tertiary homoallyl alcohols in moderate to good yield.

  4. Syntheses of 1-Aryl-5-nitro-1H-indazoles and a General One-Pot Route to 1-Aryl-1H-indazoles

    Directory of Open Access Journals (Sweden)

    Joel K. Annor-Gyamfi

    2018-03-01

    Full Text Available An efficient route to substituted 1-aryl-1H-indazoles has been developed and optimized. The method involved the preparation of arylhydrazones from acetophenone or benzaldehyde substituted by fluorine at C2 and nitro at C5, followed by deprotonation and nucleophilic aromatic substitution (SNAr ring closure in 45–90%. Modification of this procedure to a one-pot domino process was successful in the acetophenone series (73–96%, while the benzaldehyde series (63–73% required a step-wise addition of reagents. A general one-pot protocol for 1-aryl-1H-indazole formation without the limiting substitution patterns required for the SNAr cyclization has also been achieved in 62–78% yields. A selection of 1-aryl-1H-indazoles was prepared in high yield by a procedure that requires only a single laboratory operation.

  5. Mesoporous silicabis(ethylsulfanyl)propane palladium catalysts for hydrogenation and one-pot two-step Suzuki cross-coupling followed by hydrogenation.

    Science.gov (United States)

    Qazi, Asma; Sullivan, Alice

    2011-10-28

    The solid phase catalytic activity of mesoporous silicabis(ethylsulfanyl)propane palladium catalysts for hydrogenation and novel one-pot two-step Suzuki cross-coupling followed by hydrogenation is described. The efficiency of catalytic hydrogenation was measured for substrate nitrobenzene with 5, 7 and 14 nm average pore diameter materials. The 5 nm pore material performed best and was also very effective in the catalytic hydrogenation of alkene, nitrile and imine substrates. Novel one-pot two-step Suzuki cross-coupling and hydrogenation was demonstrated using bromonitro- and bromodinitrobenzene and phenylboronic acid as substrates with conversion to the corresponding coupled amino compounds. As a consequence of the high affinity of the sulfur ligands for palladium, none was detected in leaching tests and the catalyst is easily separated and recycled.

  6. One-pot synthesis of reverse type-I In2O3@In2S3 core-shell nanoparticles.

    Science.gov (United States)

    Sun, Zhaoyong; Kumbhar, Amar; Sun, Kai; Liu, Qingsheng; Fang, Jiye

    2008-04-28

    A novel method to one-pot-synthesize high-quality In(2)O(3)@In(2)S(3) core-shell nanoparticles, consisting of a step of reducing In(2)O(3) core surface into a layer of active indium metal in high-temperature organic solution and a step of converting this layer to In(2)S(3) using CS(2), has been developed.

  7. Protecting-group-free synthesis of taiwaniaquinone H using a one-pot thermal ring expansion/4π-electrocyclization strategy.

    Science.gov (United States)

    Yan, Xiuxiang; Hu, Xiangdong

    2014-06-06

    A strategy to the 6-5-6 tricyclic scaffold of taiwaniaquinoids was established on the basis of a one-pot thermal ring expansion/4π-electrocyclization process. The efficiency of this methodology has been demonstrated through its application in the total synthesis of taiwaniaquinone H, which has been accomplished in three steps and 14% overall yield in a protecting-group-free manner starting from commercially available materials.

  8. Three-component coupling of acylphosphonates and two carbonyl compounds promoted by low-valent samariums: one-Pot synthesis of beta-hydroxyphosphonates

    Science.gov (United States)

    Takaki; Itono; Nagafuji; Naito; Shishido; Takehira; Makioka; Taniguchi; Fujiwara

    2000-01-28

    Three-component coupling of acylphosphonates and two carbonyl compounds leading to beta-hydroxyphosphonates has been achieved with low-valent samariums. Thus, acylphosphonates reacted with aldehydes in the presence of semicatalytic amounts of samarium metal or SmI(2) to give acyloxyphosphonates in good yields. The second coupling reaction of the acyloxyphosphonates with aldehydes or ketones promoted by SmI(2) afforded beta-hydroxyphosphonates instead of olefins. Moreover, these two reactions could be carried out in one pot.

  9. One-pot synthesis of well-defined polyether/polyester block copolymers and terpolymers by a highly efficient catalyst switch approach

    KAUST Repository

    Alamri, Haleema

    2016-04-20

    A highly efficient methodology, based on a novel catalyst switch approach with rapid crossover characteristics, was developed for the one-pot synthesis of block co/terpolymers of cyclic ethers and esters. This new approach, which takes advantage of one of the best catalysts for epoxide (t-BuP4) and cyclic ester (t-BuP2) polymerization, opens new horizons toward the synthesis of cyclic ether/ester complex macromolecular architectures. © The Royal Society of Chemistry 2016.

  10. One pot Click chemistry: A three component reaction for the synthesis of 2-mercaptobenzimidazole linked coumarinyl triazoles as anti-tubercular agents.

    Science.gov (United States)

    Anand, Ashish; Kulkarni, Manohar V; Joshi, Shrinivas D; Dixit, Sheshagiri R

    2016-10-01

    2-Propargylthiobenzimidazole 1, 4-bromomethyl coumarins/1-aza-coumarins 2/3 and sodium azide have been reacted in one pot under Click chemistry conditions to give exclusively 1,4-disubstituted triazoles 5a-n. Anti-tubercular assays against M. tuberculosis (H37Rv) coupled with in silico molecular docking studies indicated that dimethyl substituents 5c and 5d showed promising activity with higher C-score values. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. One-pot synthesis of Pd-Pt@Pd core-shell nanocrystals with enhanced electrocatalytic activity for formic acid oxidation

    KAUST Repository

    Yuan, Qiang

    2014-01-01

    Well-defined Pd-Pt@Pd core-shell nanocrystals with a Pd-Pt alloy core and a conformal Pd shell of ~2-3 nm were directly synthesized through a one-pot, aqueous solution approach without any preformed Pd or Pt seeds. These Pd-Pt@Pd core-shell nanocrystals show an enhanced electrocatalytic activity for formic acid oxidation compared with commercial Pd black. This journal is © 2014 The Royal Society of Chemistry.

  12. Simple one-pot synthesis of platinum-palladium nanoflowers with enhanced catalytic activity and methanol-tolerance for oxygen reduction in acid media

    International Nuclear Information System (INIS)

    Zheng, Jie-Ning; He, Li-Li; Chen, Fang-Yi; Wang, Ai-Jun; Xue, Meng-Wei; Feng, Jiu-Ju

    2014-01-01

    Graphical abstract: PtPd nanoflowers were fabricated by one-pot solvothermal co-reduction method in oleylamine system, which exhibited the improved electrocatalytic activity and higher methanol tolerance for oxygen reduction, compared with commercial Pt and Pd black catalysts. - Highlights: • Bimetallic alloyed PtPd nanoflowers are prepared by a simple one-pot solvothermal co-reduction method. • PtPd nanoflowers display high catalytic performance for ORR dominated by a four-electron pathway. • PtPd nanoflowers show good methanol tolerance for ORR. - Abstract: In this work, bimetallic alloyed platinum-palladium (PtPd) nanoflowers are fabricated by one-pot solvothermal co-reduction of Pt (II) acetylacetonate and Pd (II) acetylacetonate in oleylamine system. The as-prepared nanostructures show the enhanced electrocatalytic activity for oxygen reduction reaction (ORR), dominated by a four-electron pathway based on the Koutecky-Levich plots, mainly owing to the inhibition of the formation of Pt–OH ad via the downshift of d-band center for Pt. Meanwhile, PtPd nanoflowers display good methanol tolerance and improved stability for ORR. The chronoamperometry test reveals that the current of PtPd nanoflowers remains 45.9% of its original value within 6000 s, much higher than those of commercial Pt (36.7%) and Pd (32.2%) black catalysts. Therefore, PtPd nanoflowers with unique interconnected structures can be used as a promising cathode catalyst in direct methanol fuel cells

  13. A facile one-pot Mannich reaction for the construction of fluorescent polymeric nanoparticles with aggregation-induced emission feature and their biological imaging.

    Science.gov (United States)

    Jiang, Ruming; Liu, Han; Liu, Meiying; Tian, Jianwen; Huang, Qiang; Huang, Hongye; Wen, Yuanqing; Cao, Qian-Yong; Zhang, Xiaoyong; Wei, Yen

    2017-12-01

    Multicomponent reactions (MCRs) have recently attracted great attention as one of the most important tools for the construction of various organic compounds in modern organic chemistry. In this work, we introduced an efficient one-pot strategy to successfully fabricate the fluorescent polymeric nanoparticles (FPNs) with aggregation-induced emission (AIE) characteristic via the conjugation of hyperbranched polyamino compound polyethyleneimine (PEI), AIE dye (named as PhE-OH) and paraformaldehyde (PF) through a Mannich reaction. The final amphiphilies (PEI-PF-PhE) can self-assemble into micelles in aqueous solution. We demonstrated PEI-PF-PhE FPNs showed high water dispersity, intense orange-yellow fluorescence, excellent photostability, low toxicity and high cell imaging performance. As compared with other construction strategies, the one-pot Mannich reaction possesses a number of advantages, such as simplicity, atom economy, high-efficiency and multifunctional potential. Combined with the remarkable properties of the AIE-active FPNs and the one-pot Mannich reaction, we could expect that the strategy developed in this work should be a useful tool for construction of various AIE-active functional materials for biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. One-pot synthesis of stable colloidal solutions of MFe{sub 2}O{sub 4} nanoparticles using oleylamine as solvent and stabilizer

    Energy Technology Data Exchange (ETDEWEB)

    Pérez-Mirabet, Leonardo [Departament de Química, Universitat Autònoma de Barcelona, Campus de la UAB, 08193 Bellaterra (Spain); Solano, Eduardo, E-mail: eduardo.solano@uab.cat [Departament de Química, Universitat Autònoma de Barcelona, Campus de la UAB, 08193 Bellaterra (Spain); Martínez-Julián, Fernando; Guzmán, Roger [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra (Spain); Arbiol, Jordi [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra (Spain); Institució Catalana de Recerca i Estudis Avançats (ICREA), 08019 Barcelona (Spain); Puig, Teresa; Obradors, Xavier; Pomar, Alberto [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra (Spain); Yáñez, Ramón; Ros, Josep [Departament de Química, Universitat Autònoma de Barcelona, Campus de la UAB, 08193 Bellaterra (Spain); Ricart, Susagna [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra (Spain)

    2013-03-15

    Highlights: ► One-pot synthesis of ferrite magnetic nanoparticles (<10 nm) in non-polar media. ► Nanoparticles present high monocrystal quality and monodispersion. ► Superparamagnetic behavior at room temperature. ► Nanoparticles transfer to polar media via ligand exchange. - Abstract: An easy, efficient, reproducible and scalable one-pot synthetic methodology to obtain magnetic spinel ferrite nanoparticles has been developed. This approach is based on one-pot thermal decomposition of Fe(acac){sub 3} and M(acac){sub 2} (M = Co, Mn, Cu and Zn) in oleylamine, which also acts as a capping ligand, by producing stable colloidal dispersions of nanoparticles in non-polar solvents. The properties of the nanoparticles have been studied via different techniques, such as transmission electron microscopy, which shows that nanoparticles are monocrystallines and a narrow dispersion in size; magnetic analyses have demonstrated that the resulting ferrite nanoparticles show high saturation values and superparamagnetic behavior at room temperature; X-ray diffraction has also been performed, and it confirms that the synthesized nanoparticles have a spinel structure. Complementarily, ligand exchange has been also carried out in order to produce dispersions of the synthesized nanoparticles in polar media.

  15. Modeling, Simulation, and Kinetic Studies of Solvent-Free Biosynthesis of Benzyl Acetate

    Directory of Open Access Journals (Sweden)

    Vijay Kumar Garlapati

    2013-01-01

    Full Text Available Solvent-free biosynthesis of benzyl acetate through immobilized lipase-mediated transesterification has been modeled and optimized through statistical integrated artificial intelligence approach. A nonlinear response surface model has been successfully developed based on central composite design with transesterification variables, namely, molarity of alcohol, reaction time, temperature, and immobilized lipase amount as input variables and molar conversion (% as an output variable. Statistical integrated genetic algorithm optimization approach results in an optimized molar conversion of 96.32% with the predicted transesterification variables of 0.47 M alcohol molarity in a reaction time of 13.1 h, at 37.5°C using 13.31 U of immobilized lipase. Immobilized lipase withstands more than 98% relative activity up to 6 recycles and maintains 50% relative activity until 12 recycles. The kinetic constants of benzyl acetate, namely, Km and Vmax were found to be 310 mM and 0.10 mmol h−1 g−1, respectively.

  16. Solvent-free synthesis of bacillamide analogues as novel cytotoxic and anti-inflammatory agents.

    Science.gov (United States)

    Kumar, Sunil; Aggarwal, Ranjana; Kumar, Virender; Sadana, Rachna; Patel, Bhumi; Kaushik, Pawan; Kaushik, Dhirender

    2016-11-10

    Synthesis of fourteen analogues of bacillamide, a bioactive tryptamide alkaloid of marine origin, has been accomplished through a highly efficient convergent route. The present solvent-free protocol involves the formation of thiazole ring in the initial step followed by amide coupling between substituted ethyl 2-alkyl/aryl/heteroaryl/amino/aminoarylthiazole-4-carboxylates and tryptamine in presence of 2-hydroxy-4,6-dimethylpyrimidine, a solid phase catalyst to yield N-[2-(1H-indol-3-yl)ethyl]-2-alkyl/aryl/heteroaryl/amino/aminoarylthiazole-4-carboxamides as bacillamide analogues having structural variation at position-2 of thiazole ring. Bacillamide and its analogues were evaluated for their cytotoxic activity against three cancer cell lines (HCT-116, MDA-MD-231 and JURKAT cell lines) using colorimetric cell proliferation assay. Compounds 17a and 17b exhibited potent anti-cell proliferation activity with IC50 values in the range of ∼3.0 μM and ∼0.1-0.6 μM, respectively against these cell lines. Preliminary mechanism of action studies indicates that these compounds initiate caspase dependent apoptosis. Also, compounds 16d, 16f, 17a and 17d exhibited excellent anti-inflammatory activity comparable to well-known NSAID indomethacin and better to bacillamide, when evaluated using carrageenan induced rat hind paw oedema method. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  17. Fabrication of polyacrylonitrile/ acrylamide (PAN/ AM) fibers using a solvent-free coagulation bath

    International Nuclear Information System (INIS)

    Ismail, A.F.; Mahmod, D.S.A.; Rahman, M.A.; Mustafa, A.

    2010-01-01

    Polyacrylonitrile/ Acrylamide (PAN/ AM) fibers have been produced by a simple dry-jet wet spinning process. It has been successfully carried out in the solvent-free coagulation bath. The fabrication process is focusing on controlling the formation of PAN/ AM fibers with desirable characteristics. This new approach was considered due to environmental impact of solvent usage. The production of PAN/ Am fibers consists of three main components including polyacrylonitrile (PAN), Acrylamide (AM) and dimethylformamide (DMF). Aforementioned components must be blended at a specific ratio in order to produce a homogenous polymer solution. Three polymer compositions were prepared for the PAN/ AM fibers fabrication: 16, 18 and 20 wt.%. The results showed that a semi-dilute solution (18 wt.%) was found to be the most suitable polymer composition for PAN/ AM fiber fabrication at room temperature. The PAN/ AM fibers produced at 13 degree Celsius coagulation bath temperature and residence time of 3 sec exhibited Young's modulus of 2.55 GPa which represents the highest Young modulus achieved.(author)

  18. Diffusivities, viscosities, and conductivities of solvent-free ionically grafted nanoparticles

    KAUST Repository

    Hong, Bingbing

    2013-01-01

    A new class of conductive composite materials, solvent-free ionically grafted nanoparticles, were modeled by coarse-grained molecular dynamics methods. The grafted oligomeric counterions were observed to migrate between different cores, contributing to the unique properties of the materials. We investigated the dynamics by analyzing the dependence on temperature and structural parameters of the transport properties (self-diffusion coefficients, viscosities and conductivities) and counterion migration kinetics. Temperature dependence of all properties follows the Arrhenius equation, but chain length and grafting density have distinct effects on different properties. In particular, structural effects on the diffusion coefficients are described by the Rouse model and the theory of nanoparticles diffusing in polymer solutions, viscosities are strongly influenced by clustering of cores, and conductivities are dominated by the motions of oligomeric counterions. We analyzed the migration kinetics of oligomeric counterions in a manner analogous to unimer exchange between micellar aggregates. The counterion migrations follow the "double-core" mechanism and are kinetically controlled by neighboring-core collisions. © 2013 The Royal Society of Chemistry.

  19. An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2

    Energy Technology Data Exchange (ETDEWEB)

    Motkuri, Radha K.; Vemuri, Venkata Rama S.; Barpaga, Dushyant; Schaef, Herbert T.; Loring, John S.; Martin, Paul F.; Lao, David; Nune, Satish K.; McGrail, Bernard P.

    2018-01-02

    A new efficient and solvent-free method for the synthesis of anhydrous MgCl2 from its hexahydrate is proposed. Fluidized dehydration of MgCl2·6H2O feedstock at 200 °C in a porous bed reactor yields MgCl2·nH2O (0 < n < 1), which has a similar diffraction pattern as activated MgCl2. The MgCl2·nH2O is then ammoniated directly using liquefied NH3 in the absence of solvent to form MgCl2·6NH3. Calcination of the hexammoniate complex at 300 °C then yields anhydrous MgCl2. Both dehydration and deammoniation were thoroughly studied using in situ as well as ex situ characterization techniques. Specifically, a detailed understanding of the dehydration process was monitored by in situ PXRD and in situ FTIR techniques where formation of salt with nH2O (n = 4, 2, 1, <1) was characterized. Given the reduction in thermal energy required to produce dehydrated feedstock with this method compared with current strategies, significant cost benefits are expected. Overall, the combined effect of activation, macroporosity, and coordinated water depletion allows the formation of hexammoniate without using solvent, thus minimizing waste formation.

  20. Solvent-free method for the determination of lignin-derived phenols in sediments.

    Science.gov (United States)

    Pinto, Mayara; Frena, Morgana; Dos Santos Madureira, Luiz Augusto

    2017-05-01

    A solvent-free method that uses headspace solid-phase microextraction and gas chromatography with flame ionization detection is proposed for the determination of lignin-derived phenols in sediments. The extraction and derivatization conditions for the simultaneous analysis of acetosyringone, acetovanillone, syringaldehyde, vanillin, ferulic acid, syringic acid, vanillic acid, p-hydroxybenzoic acid, and p-coumaric acid were optimized using a central composite design. After optimization, the best results were obtained with the following conditions: exposure of the polyacrylate fiber to the headspace with 60 μL of N,O-bis(trimethylsilyl)trifluoroacetamide as a derivatizing agent for 15 min and then extraction in the headspace of 100 mg of sediment (previously spiked with lignin-derived phenols) for 35 min. The accuracy of the method was estimated based on recovery tests at two concentration levels and by comparison with a high-performance liquid chromatography method reported in the literature. Based on the t-test with a confidence level of 95%, no statistical differences were observed. The detection and quantification limits for the target compounds varied according to their characteristics: values at the microgram per gram level for nonacid compounds and milligram per gram level for phenolic acids, due to the lower volatility of the derivatives. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Solid lipid nanoparticles for encapsulation of hydrophilic drugs by an organic solvent free double emulsion technique.

    Science.gov (United States)

    Becker Peres, Luana; Becker Peres, Laize; de Araújo, Pedro Henrique Hermes; Sayer, Claudia

    2016-04-01

    Encapsulation of hydrophilic compounds for drug delivery systems with high loading efficiency is not easily feasible and remains a challenge, mainly due to the leaking of the drug to the outer aqueous phase during nanoparticle production. Usually, encapsulation of hydrophilic drugs is achieved by using double emulsion or inverse miniemulsion systems that often require the use of organic solvents, which may generate toxicological issues arising from solvent residues. Herein, we present the preparation of solid lipid nanoparticles loaded with a hydrophilic compound by a novel organic solvent free double emulsion/melt dispersion technique. The main objective of this study was to investigate the influence of important process and formulation variables, such as lipid composition, surfactant type, sonication parameters and lipid solidification conditions over physicochemical characteristics of SLN dispersion. Particle size and dispersity, as well as dispersion stability were used as responses. SLN dispersions with average size ranging from 277 to 550 nm were obtained, showing stability for over 60 days at 4 °C depending on the chosen emulsifying system. Entrapment efficiency of fluorescent dyes used as model markers was assessed by fluorescence microscopy and UV-vis spectrophotometry and results suggest that the obtained lipid based nanoparticles could be potentially applied as a delivery system of water soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Natural zwitterionic l-Carnitine as efficient cryoprotectant for solvent-free cell cryopreservation.

    Science.gov (United States)

    Zhai, Hongwen; Yang, Jing; Zhang, Jiamin; Pan, Chao; Cai, Nana; Zhu, Yingnan; Zhang, Lei

    2017-07-15

    Organic solvents, such as dimethyl sulfoxide (DMSO) and glycerol, have been commonly used as cryoprotectants (CPAs) in cell cryopreservation. However, their cytotoxicity and need of complex freezing protocols have impeded their applications especially in clinical cell therapy and regenerative medicine. Trehalose has been explored as a natural CPA to cryopreserve cells, but its poor cell permeability frequently results in low cryopreservation efficacy. In this work, we presented that a natural zwitterionic molecule-l-carnitine-could serve as a promising CPA for solvent-free cryopreservation. We demonstrated that l-carnitine possessed strong ability to depress water freezing point, and with ultrarapid freezing protocol, we studied the post-thaw survival efficiency of four cell lines (GLC-82 cells, MCF-7 cells, NIH-3T3 cells and Sheep Red Blood Cells) using l-carnitine without addition of any organic solvents. At the optimum l-carnitine concentration, all four cell lines could achieve above 80% survival efficiency, compared with the significantly lower efficiency using organic CPAs and trehalose. After cryopreservation, the recovered cell behaviors including cell attachment and proliferation were found to be similar to the normal cells, indicating that the cell functionalities were not affected. Moreover, l-carnitine showed no observable cytotoxicity, which was superior to the organic CPAs. This work offered an attractive alternative to traditional CPAs and held great promise to revolutionize current cryopreservation technologies, to benefit the patients in various cell-based clinical applications. Copyright © 2017 Elsevier Inc. All rights reserved.

  3. Efficient and Highly Selective Solvent-Free Oxidation of Primary Alcohols to Aldehydes Using Bucky Nanodiamond.

    Science.gov (United States)

    Lin, Yangming; Wu, Kuang-Hsu Tim; Yu, Linhui; Heumann, Saskia; Su, Dang Sheng

    2017-09-11

    Selective oxidation of alcohols to aldehydes is widely applicable to the synthesis of various green chemicals. The poor chemoselectivity for complicated primary aldehydes over state-of-the-art metal-free or metal-based catalysts represents a major obstacle for industrial application. Bucky nanodiamond is a potential green catalyst that exhibits excellent chemoselectivity and cycling stability for the selective oxidation of primary alcohols in diverse structures (22 examples, including aromatic, substituted aromatic, unsaturated, heterocyclic, and linear chain alcohols) to their corresponding aldehydes. The results are comparable to reported transition-metal catalysts including conventional Pt/C and Ru/C catalysts for certain substrates under solvent-free conditions. The possible activation process of the oxidant and substrates by the surface oxygen groups and defect species are revealed with model catalysts, ex situ electrochemical measurements, and ex situ attenuated total reflectance. The zigzag edges of sp 2 carbon planes are shown to play a key role in these reactions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. One pot synthesis, X-ray crystal structure of 2-(2‧-hydroxyphenyl)oxazolo[4,5-b]pyridine derivatives and studies of their optical properties

    Science.gov (United States)

    Briseño-Ortega, Horacio; Juárez-Guerra, Lizbeth; Rojas-Lima, Susana; Mendoza-Huizar, Luis Humberto; Vázquez-García, Rosa A.; Farfán, Norberto; Arcos-Ramos, Rafael; Santillan, Rosa; López-Ruiz, Heralio

    2018-04-01

    A series of five 2-(2-hydroxyphenyl)oxazolo [4,5-b]pyridines (HPOP) (3a-e), where four are novel, were synthesized by a mild, one pot, phenylboronic acid-NaCN catalyzed reaction. Spectroscopic characterization and photophysical properties of these compounds are reported. Absorption and excitation spectra of the compounds were dependent on the substituents in the phenyl ring. Fluorescence quantum yields (0.009-0.538) were associated with the donor strength and the position of the substituents. Also, DFT analysis allowed us to determine the contribution of diethylamino and methoxy moieties to the π-system, which is in agreement with the experimental data analyzed in solution and by cyclic voltammetry. The results obtained in the solid state by single-crystal X-ray diffraction experiments indicate that, the quasi-planarity envisioned for the explored compounds is present, supporting the hypothesis that both the H-bonding of a hydroxyl group to the Cdbnd N moiety and a donor groups such as diethylamino and methoxy moieties favor an electronic communication. Due to the facile synthesis and their photophysical properties, the novel HPOP 3a-e have potential application as organic semiconductors.

  5. Structure of the Dioxygenase AsqJ: Mechanistic Insights into a One-Pot Multistep Quinolone Antibiotic Biosynthesis

    KAUST Repository

    Bräuer, Alois

    2015-11-10

    © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. Multienzymatic cascades are responsible for the biosynthesis of natural products and represent a source of inspiration for synthetic chemists. The FeII/α-ketoglutarate-dependent dioxygenase AsqJ from Aspergillus nidulans is outstanding because it stereoselectively catalyzes both a ferryl-induced desaturation reaction and epoxidation on a benzodiazepinedione. Interestingly, the enzymatically formed spiro epoxide spring-loads the 6,7-bicyclic skeleton for non-enzymatic rearrangement into the 6,6-bicyclic scaffold of the quinolone alkaloid 4′-methoxyviridicatin. Herein, we report different crystal structures of the protein in the absence and presence of synthesized substrates, surrogates, and intermediates that mimic the various stages of the reaction cycle of this exceptional dioxygenase.

  6. Optimization of the production of biodiesel by a commercial immobilized lipase in a solvent-free system using a response surface methodology

    Directory of Open Access Journals (Sweden)

    ZORICA KNEZEVIC

    2008-02-01

    Full Text Available Response surface methodology was used for the evaluation of the effects of various factors on the synthesis of biodiesel catalyzed with immobilized lipase from Rhizomucor miehei in a solvent-free system. The production of biodiesel was optimized and model response equations were obtained, enabling the prediction of biodiesel production from the values of the four main factors. It would seem that the reaction temperature and the amount of water predominantly determined the conversion process while the methanol/oil molar ratio had no significant influence on the reaction rate. The temperature and amount of water showed negative interactive effects on the observed reaction rate per amount of enzyme. However, there were no significant interactions among the other variables according to the test of statistical significance. The highest yield of 10.15 mol kg-1 enzyme was observed at 45 °C with a 6:1 methanol to oil molar ratio and with no added water in the system.

  7. Greening Wittig Reactions: Solvent-Free Synthesis of Ethyl Trans-Cinnamate and Trans-3-(9-Anthryl)-2-Propenoic Acid Ethyl Ester

    Science.gov (United States)

    Nguyen, Kim Chi; Weizman, Haim

    2007-01-01

    Green procedure is used to create solvent-free alternatives for conventional Wittig reactions, which are widely used to install a double bond in a highly selective manner. Solvent-free reactions reduce health and environmental risks and provide a basis for an inquiry-based discussion of the stereochemistry of the Wittig reaction and the factors…

  8. One-pot cascade michael.cyclization reactions of ο-hydroxycinnamaldehydes: Synthesis of functionalized 2,3-dihydrobenzofuranes

    Energy Technology Data Exchange (ETDEWEB)

    Gwon, Sung Hyuk; Kim, Sunggon [Kyonggi Univ., Suwon (Korea, Republic of)

    2012-04-15

    We described the cascade Michael.cyclization reaction of o-hydroxycinnamaldehydes with diethyl α-bromomalonate promoted by potassium carbonate. The reactions provided functionalized 2,3-dihydrobenzofurans in good yields for a variety of o-hydroxyaromatic α,β-unsaturated aldehydes. Current work focuses on expanding the scope of this reaction to other substrates such as sulfur yields, and on developing an efficient catalytic asymmetric variant. 2,3-Dihydrobenzofurans are found in numerous biologically active natural products and synthetic compounds. These are an attractive type of oxygenated compound because their basic core skeleton is present in neolignans, pterocarpans, and synthetic drugs used in the treatment of pulmonary hypertension, atherosclerotic peripheral arterial disease, and central nervous system trauma and ischemia. Owing to the importance of their structures, numerous synthetic methods for 2,3-dihydrobenzofurans have been developed, primarily: radical cyclizations, Lewis acid promoted reactions, anionic cyclizations, and transition-metal catalyzed processes. However, these methods cannot be generalized as much as is desirable, and they yielded poor chemo- and/or stereoselectivities. Hence, the development of an efficient enantioselective synthetic method for obtaining 2,3-dihydrobenzofuran scaffolds attracted our attention.

  9. One-pot cascade michael.cyclization reactions of ο-hydroxycinnamaldehydes: Synthesis of functionalized 2,3-dihydrobenzofuranes

    International Nuclear Information System (INIS)

    Gwon, Sung Hyuk; Kim, Sunggon

    2012-01-01

    We described the cascade Michael.cyclization reaction of o-hydroxycinnamaldehydes with diethyl α-bromomalonate promoted by potassium carbonate. The reactions provided functionalized 2,3-dihydrobenzofurans in good yields for a variety of o-hydroxyaromatic α,β-unsaturated aldehydes. Current work focuses on expanding the scope of this reaction to other substrates such as sulfur yields, and on developing an efficient catalytic asymmetric variant. 2,3-Dihydrobenzofurans are found in numerous biologically active natural products and synthetic compounds. These are an attractive type of oxygenated compound because their basic core skeleton is present in neolignans, pterocarpans, and synthetic drugs used in the treatment of pulmonary hypertension, atherosclerotic peripheral arterial disease, and central nervous system trauma and ischemia. Owing to the importance of their structures, numerous synthetic methods for 2,3-dihydrobenzofurans have been developed, primarily: radical cyclizations, Lewis acid promoted reactions, anionic cyclizations, and transition-metal catalyzed processes. However, these methods cannot be generalized as much as is desirable, and they yielded poor chemo- and/or stereoselectivities. Hence, the development of an efficient enantioselective synthetic method for obtaining 2,3-dihydrobenzofuran scaffolds attracted our attention

  10. Extraction of orange peel's essential oil by solvent-free microwave extraction

    Science.gov (United States)

    Qadariyah, Lailatul; Amelia, Prilia Dwi; Admiralia, Cininta; Bhuana, Donny S.; Mahfud, Mahfud

    2017-05-01

    Sweet orange peel (Citrus sinensis) is part of orange plant that contains essential oils. Generally, taking essential oil from orange peel is still using hydrodistillation and steam-hydrodistillation method which still needs solvent and takes a long time to produce high quality essential oil. Therefore, the objectives of this experiment are to study the process of orange peel's essential oil extraction using Solvent Free Microwave Extraction (SFME) and to study the operating condition that effect an optimum yield and quality of the essential oil. In this experiment, extraction process with SFME method goes for 60 minutes at atmospheric pressure. Variables for SFME are: variation of orange peel condition (fresh and dry), ratio orange peel mass to distiller volume (0,1; 0,2; 0,3; 0,4 g/mL), orange peel size (±0,5; ±2; ±3,5 cm width), and microwave power (100, 264, 400 Watt). Moisture content of fresh peel is 71,4% and for dry peel is 17,37% which is obtained by sun drying. The result of this experiment will be analyzed with GC-MS, SEM, density, and miscibility in ethanol 90%. The optimum result obtained from this experiment based on the number of the yield under condition of fresh orange peel is at peel mass/distiller volume 0,1 g/mL, orange peel size ±3,5 cm width, and microwave power 400 Watt, results 1,6738% yield. The result of GC-MS for fresh orange peel shows that the dominant compound is Limonene 54,140% and for dry orange peel is Limonene 59,705%. The density obtained is around 0,8282-0,8530 g/mL and miscibility in ethanol 90% is 1:5.

  11. Solvent free synthesis and structural evaluation of polyurethane films based on poly(ethylene glycol and poly(caprolactone

    Directory of Open Access Journals (Sweden)

    V. Kupka

    2016-06-01

    Full Text Available Biodegradable amphiphilic polyurethane films (bio-PUs were synthesized by solvent free polyaddition reaction of hydrophilic poly(ethylene glycol (PEG and hydrophobic poly(caprolactone (PCL as macrodiols with hexamethylene diisocyanate. Samples were subsequently heat cured in order to obtain 3D crosslinked structure. Different PCL/PEG ratios allowed controlling the toughness of the resulting bio-PUs. Significant enhancement of Young’s modulus, strength and elongation at break was observed at a PCL/PEG molar ratio above 3. The change in the bio-PU mechanical behavior was ascribed to the formation of crystalline PCL domains in the bio-PU network. The presence of PEG increased both the ability to absorb water and the rate of hydrolytic degradation, while PCL increased the cell viability. Prepared solvent free bio-PUs may advantageously be used in medicine as elastic resorbable material applicable against post-surgical adhesions.

  12. Application of 2k Full Factorial Design in Optimization of Solvent-Free Microwave Extraction of Ginger Essential Oil

    Directory of Open Access Journals (Sweden)

    Mumtaj Shah

    2014-01-01

    Full Text Available The solvent-free microwave extraction of essential oil from ginger was optimized using a 23 full factorial design in terms of oil yield to determine the optimum extraction conditions. Sixteen experiments were carried out with three varying parameters, extraction time, microwave power, and type of sample for two levels of each. A first order regression equation best fits the experimental data. The predicted values calculated by the regression model were in good agreement with the experimental values. The results showed that the extraction time is the most prominent factor followed by microwave power level and sample type for extraction process. An average of 0.25% of ginger oil can be extracted using current setup. The optimum conditions for the ginger oil extraction using SFME were the extraction time 30 minutes, microwave power level 640 watts, and sample type, crushed sample. Solvent-free microwave extraction proves a green and promising technique for essential oil extraction.

  13. Application of 2k Full Factorial Design in Optimization of Solvent-Free Microwave Extraction of Ginger Essential Oil

    OpenAIRE

    Shah, Mumtaj; Garg, S. K.

    2014-01-01

    The solvent-free microwave extraction of essential oil from ginger was optimized using a 23 full factorial design in terms of oil yield to determine the optimum extraction conditions. Sixteen experiments were carried out with three varying parameters, extraction time, microwave power, and type of sample for two levels of each. A first order regression equation best fits the experimental data. The predicted values calculated by the regression model were in good agreement with the experimental ...

  14. Synthesis of Substituted 2,2′-Dinitrobiphenyls by a Novel Solvent-Free High Yielding Ullmann Coupling Biarylation

    OpenAIRE

    Epps, Ayunna; Barbas, John; Mandouma, Ghislain

    2014-01-01

    Solvent-free reaction using a high-speed ball milling technique has been applied to the classical Ullmann coupling reaction for the first time. Biarylation of 2-iodonitrobenzene was achieved in quantitative yield when performed in a custom-made copper vial through continuous shaking without additional copper or solvent. The product was solid, NMR ready and required no lengthy extraction for purification. This reaction was cleaner, and faster than solution phase coupling which requires longer ...

  15. Solvent-Free Off-On Detection of the Improvised Explosive Triacetone Triperoxide (TATP) with Fluorogenic Materials.

    Science.gov (United States)

    Calvo-Gredilla, Patricia; García-Calvo, José; Cuevas, José V; Torroba, Tomás; Pablos, Jesús-Luis; García, Félix C; García, José-Miguel; Zink-Lorre, Nathalie; Font-Sanchis, Enrique; Sastre-Santos, Ángela; Fernández-Lázaro, Fernando

    2017-10-09

    A fluorogenic perylenediimide-functionalized polyacrylate capable of generating color and fluorescence changes in the presence of triacetone triperoxide TATP), an improvised explosive used in terrorist attacks, under solvent-free, solid-state conditions has been developed. The material works by accumulating volatile TATP until it reaches a threshold; therefore, triggering colorimetric and fluorescent responses. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. An Organocatalyzed and Ultrasound Accelerated Expeditious Synthetic Route to 1,5-Benzodiazepines under Solvent-Free Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Shinde, Pravin V.; Shingate, Bapurao B.; Shingare, Murlidhar S. [Babasaheb Ambedkar Marathwada University, Aurngabad (India)

    2011-04-15

    In the present work, successful implementation of ultrasound irradiations for the rapid synthesis of 1,5- benzodiazepine derivatives under solvent-free conditions is demonstrated. Use of a novel catalyst i.e. camphor sulphonic acid in combination with ultrasound technique is reported for the first time. Comparative study for the synthesis of 1,5-benzodiazepines using conventional as well as ultrasonication method is discussed.

  17. NaHSO4-SiO2-Promoted Solvent-Free Synthesis of Benzoxazoles, Benzimidazoles, and Benzothiazole Derivatives

    Directory of Open Access Journals (Sweden)

    K. Ravi Kumar

    2013-01-01

    Full Text Available An efficient protocol has been developed for the preparation of a library of benzoxazole, benzimidazole, and benzothiazole derivatives from reactions of acyl chlorides with o-substituted aminoaromatics in the presence of catalytic amount of silica-supported sodium hydrogen sulphate under solvent-free conditions. Simple workup procedure, high yield, easy availability, reusability, and use of ecofriendly catalyst are some of the striking features of the present protocol.

  18. Dumbbell-like ZnO nanoparticles-CeO2 nanorods composite by one-pot hydrothermal route and their electrochemical charge storage

    International Nuclear Information System (INIS)

    He, Geping; Fan, Huiqing; Ma, Longtao; Wang, Kaige; Liu, Chao; Ding, Donghai; Chen, Li

    2016-01-01

    Graphical abstract: Dumbbell-like ZnO nanoparticles-CeO 2 nanorods (ZnONPs-CeO 2 NRs) composite with superior electrochemical performance was fabricated by one-pot hydrothermal process. Charge storage of the ZnONPs-CeO 2 NRs composite was more 12 times than its precursor CeO 2 NRs. - Highlights: • ZnONPs-CeO 2 NRs composite fabricated by one-pot hydrothermal growth owns dumbbell structure. • ZnO nanoparticles in situ anchor on the surface of CeO 2 nanorods. • Formation mechanism of dumbbell-structured ZnONPs-CeO 2 NRs composite is offered. • Relevance between structural features and properties of EIS, CV, GCD is displayed. • Calcined ZnONPs-CeO 2 NRs composite as electrode material benefits super-capacitor charge storage. - Abstract: Dumbbell-like ZnO nanoparticles-CeO 2 nanorods (ZnONPs-CeO 2 NRs) composites with superior electrochemical performance were fabricated by one-pot hydrothermal process and characterized by X-ray diffraction, an energy dispersive spectrum, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and nitrogen adsorption–desorption isotherms. The ZnONPs-CeO 2 NRs nanostructure possessed larger Brunauer–Emmett–Teller (BET) surface, crystallinity, lower resistance. The specific capacitance of ZnONPs-CeO 2 NRs composite (162.08 mF g −1 ) was higher than that of precursor CeO 2 NRs (151.43 mF g −1 ) in galvanostatic charge/discharge, and the super-capacitor charge storage of ZnONPs-CeO 2 NRs (581.39 F g −1 ) was more 12 times than the precursor (46.63 F g −1 ). The improved electrochemical performances could be ascribed to the import of ZnONPs, which induced variations in the structure, conductivity and surface morphology.

  19. Fully automated one-pot two-step synthesis of 4-[(18)F]-ADAM, a potent serotonin transporter imaging agent.

    Science.gov (United States)

    Cheng, Cheng-Yi; Chou, Ta-Kai; Shiue, Chyng-Yann

    2016-04-01

    N,N-dimethyl-2-(2-amino-4-[(18)F]fluorophenylthio)benzylamine (4-[(18)F]-ADAM, 2) is a potent serotonin transporter (SERT) imaging agent. In order to fulfill the demand of clinical studies, we have developed a fully automated one-pot two-step synthesis of this potent SERT imaging agent. The 4-[(18)F]-ADAM (2) was synthesized using a commercially available GE TRACERlab FN module. Briefly, the precursor, N,N-dimethyl-2-(2,4-dinitrophenylthio) benzylamine (1) in DMSO was reacted with K[(18)F]/K2.2.2 in a glassy carbon reaction vessel at 120°C for 7.5min followed by reduction of the intermediate with NaBH4/Cu(OAc)2 in EtOH in the same vessel at 80°C for 20min. The reaction mixture was then purified with high-performance liquid chromatography (HPLC) and solid phase extraction (SPE) to give (2). The quality of (2) synthesized by this method was verified by HPLC and TLC as compared to its authentic sample synthesized by two-pot two-step method. Using this automated one-pot two-step method, the radiochemical yield (RCY) of (2) was 2.5±0.8% (n=12, EOS) in a synthesis time of 100±6min from EOB with a specific activity of 4.4±1.9Ci/μmol (n=12, EOS). Radioligand (2) was stable over 4h at room temperature. This fully automated one-pot two-step synthetic method using a commercially available GE TRACERlab FN module could simplify the synthesis of 4-[(18)F]-ADAM (2) and fulfill its demand for both animal and human studies, especially for study sites without a cyclotron. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. A novel one-pot process for near-net-shape fabrication of open-porous resorbable hydroxyapatite/protein composites and in vivo assessment

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Berit, E-mail: beritm@uni-bremen.de [University of Bremen, Advanced Ceramics, Am Biologischen Garten 2, 28359 Bremen (Germany); Koch, Dietmar, E-mail: dietmar.koch@dlr.de [German Aerospace Center, Ceramic Composite Structures, Pfaffenwaldring 38-40, 70569 Stuttgart (Germany); Lutz, Rainer, E-mail: rainer.lutz@uk-erlangen.de [University of Erlangen-Nuremberg, Department of Oral and Maxillofacial Surgery, Glueckstrasse 11, 91054 Erlangen (Germany); Schlegel, Karl A., E-mail: andreas.schlegel@uk-erlangen.de [University of Erlangen-Nuremberg, Department of Oral and Maxillofacial Surgery, Glueckstrasse 11, 91054 Erlangen (Germany); Treccani, Laura, E-mail: treccani@uni-bremen.de [University of Bremen, Advanced Ceramics, Am Biologischen Garten 2, 28359 Bremen (Germany); Rezwan, Kurosch, E-mail: krezwan@uni-bremen.de [University of Bremen, Advanced Ceramics, Am Biologischen Garten 2, 28359 Bremen (Germany)

    2014-09-01

    We present a mild one-pot freeze gelation process for fabricating near-net, complex-shaped hydroxyapatite scaffolds and to directly incorporate active proteins during scaffold processing. In particular, the direct protein incorporation enables a simultaneous adjustment and control of scaffold microstructure, porosity, resorbability and enhancement of initial mechanical and handling stability. Two proteins, serum albumin and lysozyme, are selected and their effect on scaffold stability and microstructure investigated by biaxial strength tests, electron microscopy, and mercury intrusion porosimetry. The resulting hydroxyapatite/protein composites feature adjustable porosities from 50% to 70% and a mechanical strength ranging from 2 to 6 MPa comparable to that of human spongiosa without any sintering step. Scaffold degradation behaviour and protein release are assessed by in vitro studies. A preliminary in vivo assessment of scaffold biocompatibility and resorption behaviour in adult domestic pigs is discussed. After implantation, composites were resorbed up to 50% after only 4 weeks and up to 65% after 8 weeks. In addition, 14% new bone formation after 4 weeks and 37% after 8 weeks were detected. All these investigations demonstrate the outstanding suitability of the one-pot-process to create, in a customisable and reliable way, biocompatible scaffolds with sufficient mechanical strength for handling and surgical insertion, and for potential use as biodegradable bone substitutes and versatile platform for local drug delivery. - Highlights: • We present a one-pot process for directly incorporating protein into HAp scaffolds. • The effect of two model proteins, BSA and LSZ, on scaffold properties is analysed. • HAp/protein scaffolds feature a mechanical strength comparable to human spongiosa. • BSA incorporation in scaffolds leads to strength increase despite porosity increment. • New bone formation in-vivo exceeds established xenograft bone substitutes.