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Sample records for catalyzed solvent-free one-pot

  1. Oxalic acid catalyzed solvent-free one pot synthesis of coumarins

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Oxalic acid was found to be an efficient catalyst for Pechmann condensation, which includes the reaction between phenols and β-keto esters leading to formation of coumarin derivatives. The advantages of present methods are the use of cheap and easy available catalyst, solvent-free reaction conditions, better yields and shorter reaction time.

  2. One-pot synthesis of 1-amidoalkyl-2-naphthols catalyzed by melamine-Br3 under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Arash Ghorbani-Choghamarani; Shima Rashidimoghadam

    2014-01-01

    A facile and efficient method has been developed for the synthesis of 1-amidoalkyl-2-naphthols via the one-pot multi-component condensation of 2-naphthol with aromatic aldehydes and acetamide or thioacetamide in the presence of melamine-Br3 under solvent-free conditions. There are several advantages to this reaction, including high yields, short reaction time, and high catalytic efficiency.

  3. N-Bromosuccinimide Catalyzed One-pot and Rapid Synthesis of Acetamidobenzyl Naphthols under Mild and Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    SHATERIAN Hamid Reza; YARAHMADI Hossein; GHASHANG Majid; SAFARI MEHMANDOSTI Moharram

    2008-01-01

    An efficient,facile and expeditious direct protocol for the preparation of acetamidobenzyl naphthols employing a multi-component and one-pot condensation reaction of 2-naphthoi,benzaldehydes,and acetamide in the presence of N-bromosuccinimide(NBS)under thermal and microwave irradiation conditions has been described.The present protocol with NBS catalyst is convincingly superior to the recently reported catalytic methods.

  4. Efficient Magnesium Bromide-Catalyzed One-pot Synthesis of Substituted 1,2,3,4-Tetrahydropyrimidin-2-ones Under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    沙里海·H; 郭庆祥

    2005-01-01

    An efficient and environmentally friendly procedure for the one-pot synthesis of tetrahydropyrimidinones from aldehydes, β-diketones and urea/thiourea by using magnesium bromide as an inexpensive and easily available catalyst under solvent-free conditions was described. Compared with the classical Biginelli reaction conditions, this new method has the advantage of good to excellent yields (74%-94%) and short reaction time (45-90 min). The structure of the Biginelli reaction product from β-diketone, salicylaldehyde and urea has been proposed to possess an oxygen-bridge by cyclization (intramolecular Michael-addition).

  5. 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

    OpenAIRE

    Vahid Vahabi; Farhad Hatamjafari

    2014-01-01

    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 environ...

  6. 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.

  7. An Efficient One-Pot Synthesis of Dihydropyrimidinones Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Farhad Hatamjafari

    2014-03-01

    Full Text Available An efficient method for one-pot synthesis of 3,4-Dihydropyrimidin-2-(1H -one derivatives the Biginelli condensation reaction of aromaticaldehydes, β-ketoesters and urea under solvent-free conditions was described.

  8. 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.

  9. One-pot Solvent-free Catalytic Dimerization Reaction of Phenylacetylene to 1-Phenylnaphthalene

    Indian Academy of Sciences (India)

    Avat (Arman) Taherpour; Sepehr Taban; Ako Yari

    2015-09-01

    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 barrier around C-C of the phenyl and naphthalene parts of the molecule and its UV-Visible spectrum were calculated. The modelling of the mechanism of production of 2 from 1 was performed with and without Cu/C catalyst. The data of EDS and SEM of the Cu/C catalyst surface are also reported.

  10. Facile solvent-free one-pot synthesis of pyranobenzopyrans and their derivatives

    Indian Academy of Sciences (India)

    P Sirisha; Suhas Pednekar; Nant R Kapdi; Minal Naik

    2011-09-01

    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.

  11. A SIMPLE, EFFICIENT AND SOLVENT FREE ONE POT SYNTHESIS OF 3, 3 DIHETEROAROMATIC OXINDOLE

    Directory of Open Access Journals (Sweden)

    Syed Shahed Ali

    2013-04-01

    Full Text Available Formic acid catalyzed, single step and environmentally friendly process for synthesis of 3, 3- diheteroaromatic oxindole derivatives is described. This adopted protocol for Friedel- Crafts substitution reaction has the advantage of reusability of the catalyst, high yields and ease of separation of pure products.

  12. Covalently anchored sulfonic acid on silica gel (SiO2-R-SO3H) as an efficient and reusable heterogeneous catalyst for the one-pot synthesis of 1,8-dioxooctahydroxanthenes under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Gholam Hossein Mahdavinia; Mohammad A.Bigdeli; Yaser Saeidi Hayeniaz

    2009-01-01

    A highly efficient one-pot synthesis of 1,8-dioxooctahydroxanthenes under solvent-free conditions catalyzed by sulfonic acid covalently anchored onto the surface of silica gel is reported.All types of aldehydes,including aromatic,unsaturated,and heterocyclic,are used.The silica gel/sulfonic acid catalyst (SiO2-R-SO3H) is completely heterogeneous and can be recycled.

  13. One-Pot Synthesis of 2-Phenylimidazo[1,2-α]pyridines from Acetophenone, [Bmim]Br3 and 2-Aminopyridine under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Jian-Ping Xu

    2012-11-01

    Full Text Available One-pot synthesis of 2-phenylimidazo[1,2-α]pyridines from acetophenone, [Bmim]Br3 and 2-aminopyridine under solvent-free conditions in the presence of Na2CO3, gave the corresponding 2-phenylimidazo[1,2-α]pyridines in excellent yields ranging from 72% to 89%.

  14. A novel and an efficient catalyst for one-pot synthesis of 2,4,5-trisubstituted imidazoles by using microwave irradiation under solvent-free conditions

    Indian Academy of Sciences (India)

    Javad Safari; Shiva Dehghan Khalili; Sayed Hossein Banitaba

    2010-05-01

    (NH4)6Mo7O24.4H2O has been used as an efficient catalyst for an improved and rapid synthesis of 2,4,5-trisubstituted imidazoles by a three-component, one-pot condensation of benzil, aryl aldehydes and ammonium acetate in good yields under solvent-free conditions using microwave irradiation. The reactions in conventional heating conditions were compared with the microwave-assisted reactions.

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

    OpenAIRE

    Siddiqui, Bina S.; Syed Imran Hassan; Farhat Farhat; Syed Nawazish Ali; Sabira Begum

    2008-01-01

    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 ...

  16. 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.

  17. One-pot synthesis of tri-and tetra-substituted imidazoles using sodium dihydrogen phosphate under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Zahed Karimi-Jaberi; Mohammad Barekat

    2010-01-01

    Sodium dihydrogen phosphate (NaH2PO4) efficiently catalyzes the condensation reaction of benzil,aldehydes,amines and ammonium acetate in a four-component reaction under solvent-free conditions.The reaction proceeds rapidly and affords the corresponding tetra-substituted imidazoles in high yields.Also an efficient route was developed for the synthesis of tri-substituted imidazoles from condensation of benzil,aldehydes and ammonium acetate using NaH2PO4.

  18. Cerium (IV) sulfate:A highly efficient reusable heterogeneous catalyst for the one-pot synthesis of 2,3-dihydroquinazolin-4(1H)-ones under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Abolghasem Davoodnia; Maryam Khashi; Niloofar Tavakoli-Hoseini

    2014-01-01

    Cerium (IV) sulfate tetrahydrate, Ce(SO4)2·4H2O, is a novel inorganic solid acidic catalyst that effi-ciently catalyzes the synthesis of 2,3-dihydroquinazolin-4(1H)-ones via the one-pot three- compo-nent reaction of isatoic anhydride, aromatic aldehydes, and a nitrogen source (ammonium acetate, ammonium carbonate, ammonium chloride, or methylamine) under solvent-free conditions. The desired products are obtained in short reaction time with high yields. The catalyst is inexpensive and readily available and can be recovered conveniently and reused such that considerable catalytic activity can still be achieved after the fifth run. Easy work-up and avoiding the use of harmful or-ganic solvents are other advantages of this simple procedure.

  19. Lithium-Acetate-Mediated Biginelli One-Pot Multicomponent Synthesis under Solvent-Free Conditions and Cytotoxic Activity against the Human Lung Cancer Cell Line A549 and Breast Cancer Cell Line MCF7

    Directory of Open Access Journals (Sweden)

    Harshita Sachdeva

    2012-01-01

    Full Text Available Various Biginelli compounds (dihydropyrimidinones have been synthesized efficiently and in high yields under mild, solvent-free, and eco-friendly conditions in a one-pot reaction of 1,3-dicarbonyl compounds, aldehydes, and urea/thiourea/acetyl thiourea using lithium-acetate as a novel catalyst without the addition of any proton source. Comparative catalytic efficiency of lithium-acetate and polyphosphoric acid to catalyze Biginelli condensation is also studied under neat conditions. The reaction is carried out in the absence of any solvent and represents an improvement of the classical Biginelli protocol and an advantage in comparison with FeCl3·6H2O, NiCl2·6H2O and CoCl2·6H2O that were used with HCl as a cocatalyst. Compared to classical Biginelli reaction conditions, the present method has advantages of good yields, short reaction times, and experimental simplicity. The obtained products have been identified by spectral (1H NMR and IR data and their melting points. The prepared compounds are evaluated for anticancer activity against two human cancer cell lines (lung cancer cell line A549 and breast cancer cell line MCF7.

  20. Mesostructured SBA-15-Pr-SO3H: An efficient solid acid catalyst for one-pot and solvent-free synthesis of 3,4-dihydro-2-pyridone derivatives

    Indian Academy of Sciences (India)

    Ghodsi Mohammadi Ziarani; Somayeh Mousavi; Negar Lashgari; Alireza Badiei

    2013-11-01

    3,4-Dihydro-2-pyridone derivatives have been prepared efficiently via a one-pot four-component reaction of benzaldehyde derivatives, Meldrum’s acid, methyl acetoacetate and ammonium acetate in the presence of sulphonic acid-functionalized ordered nanoporous SBA-15 as a nano heterogeneous catalyst under solvent-free conditions. This process is a simple, environmentally friendly, rapid and high yielding reaction.

  1. Boric acid as a mild and efficient catalyst for one-pot synthesis of 1-amidoalkyl-2-naphthols under solvent-free conditions

    Indian Academy of Sciences (India)

    Aziz Shahrisa; Somayeh Esmati; Mahdi Gholamhosseini Nazari

    2012-07-01

    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.

  2. Lewis acidic (choline chloride.3ZnCl2) ionic liquid: A green and recyclable catalyst for the one-pot synthesis of 4-((3-indolyl)(aryl)methyl)-N,N-dimethylanilines under solvent-free conditions

    Indian Academy of Sciences (India)

    Rahim Hekmatshoar; Farnoush Mousavizadeh; Reyhaneh Rahnamafar

    2013-09-01

    A green and convenient procedure for the one-pot multicomponent synthesis of 4-((3-indolyl)(aryl)methyl)-N,N-dimethylanilines using (choline chloride.3ZnCl2) ionic liquid as catalyst, at 100°C and under solvent-free condition is described. Utilizing environmentally benign reagents, elimination of organic solvents, enhanced rates, reusability and moisture stability of the catalyst are the remarkable features observed in the reported reaction system. The catalyst was recycled up to four times with no noticeable drop in activity.

  3. 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.

  4. An efficient Biginelli one-pot synthesis of new benzoxazole-substituted dihydropyrimidinones and thiones catalysed by trifluoro acetic acid under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    D.Shobha; M.Adharvana Chari; K.H.Ahn

    2009-01-01

    An efficient synthesis of benzoxazole-substituted 3,4-dihydropyrimidinones(DHPMs)using trifluoro acetic acid as the catalyst for the first time from an aldehyde,β-keto ester and benzoxazole-substituted urea/thiourea under solvent-free conditions is described.Compared to the classical Biginelli reaction conditions,this new method consistently has the advantage of excellent yields(80-91%)and short reaction time(40-130 min)at reflux temperature.

  5. Transition metal-catalyzed one-pot synthesis of water-soluble dendritic molecular nanocarriers.

    Science.gov (United States)

    Chen, Guanghui; Guan, Zhibin

    2004-03-10

    Here, we report the first example of transition metal-catalyzed one-pot synthesis of water-soluble dendritic molecular nanocarriers behaving like unimolecular micelles. Using the palladium-alpha-diimine chain walking catalyst, copolymerization of ethylene and comonomer 3 afforded, in one step, amphiphilic copolymer 1 having a hydrophobic core and a hydrophilic shell. A much larger amphiphilic core-shell copolymer 2 was synthesized by a two-step approach: a copolymer having many free hydroxyl groups was first prepared, which was subsequently coupled to poly(ethylene glycol) (PEG) to afford the copolymer 2. Light-scattering, fluorescence, and UV/vis spectroscopic studies with Nile Red in aqueous solution showed unimolecular micellar properties for both copolymers 1 and 2. The dye encapsulation capacity for the core-shell copolymers is nearly proportional to the molecular weight of the hydrophobic core. The unimolecular micellar properties coupled with the good water solubility and biocompatibility of the PEG moieties make these molecular nanocarriers promising candidates for many applications including drug delivery and controlled drug release. PMID:14995158

  6. 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.

  7. Facile Synthesis of Symmetrical Triindolylmethanes Catalyzed by Iodine under Solvent-free Condition

    Institute of Scientific and Technical Information of China (English)

    ZENG Xiao-Fei; JI Shun-Jun; SU Xiao-Ming

    2008-01-01

    The reaction of various indoles (1a-1k, 3 equiv.) with triethyl orthoformate (1.2 equiv.) catalyzed by I2 (5mol%) at room temperature in 2-15 min under a solvent-free condition afforded the respective symmetrical triindolylmethanes (3a-3k) in good to excellent yields without any side products.

  8. Titanium-catalyzed multicomponent couplings: efficient one-pot syntheses of nitrogen heterocycles.

    Science.gov (United States)

    Odom, Aaron L; McDaniel, Tanner J

    2015-11-17

    Nitrogen-based heterocycles are important frameworks for pharmaceuticals, natural products, organic dyes for solar cells, and many other applications. Catalysis for the formation of heterocyclic scaffolds, like many C-C and C-N bond-forming reactions, has focused on the use of rare, late transition metals like palladium and gold. Our group is interested in the use of Earth-abundant catalysts based on titanium to generate heterocycles using multicomponent coupling strategies, often in one-pot reactions. To be of maximal utility, the catalysts need to be easily prepared from inexpensive reagents, and that has been one guiding principle in the research. For this purpose, a series of easily prepared pyrrole-based ligands has been developed. Titanium imido complexes are known to catalyze the hydroamination of alkynes, and this reaction has been used to advantage in the production of α,β-unsaturated imines from 1,3-enynes and pyrroles from 1,4-diynes. Likewise, catalyst design can be used to find complexes applicable to hydrohydrazination, coupling of a hydrazine and alkyne, which is a method for the production of hydrazones. Many of the hydrazones synthesized are converted to indoles through Fischer cyclization by addition of a Lewis acid. However, more complex products are available in a single catalytic cycle through coupling of isonitriles, primary amines, and alkynes to give tautomers of 1,3-diimines, iminoamination (IA). The products of IA are useful intermediates for the one-pot synthesis of pyrazoles, pyrimidines, isoxazoles, quinolines, and 2-amino-3-cyanopyridines. The regioselectivity of the reactions is elucidated in some detail for some of these heterocycles. The 2-amino-3-cyanopyridines are synthesized through isolable intermediates, 1,2-dihydro-2-iminopyridines, which undergo Dimroth rearrangement driven by aromatization of the pyridine ring; the proposed mechanism of the reaction is discussed. The IA-based heterocyclic syntheses can be accomplished

  9. Efficient One-pot Synthesis of 12-Aryl-8, 9, 10, 12-tetrahydrobenzo[a]xanthen-11-ones Under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    JIA Xu-dong; HAN Song-yang; DUAN Hai-feng; LIN Ying-jie; CAO Jun-gang; LIANG Da-peng; WU Mao-cheng

    2013-01-01

    Multi-component condensation of 2-naphthol,aromatic aldehydes,and cyclic 1,3-dicarbonyl compounds catalyzed by ionic liquid [NSPTEA][HSO4] was accomplished for the synthesis of a series of 12-aryl-8,9,10,12-tetrahydrobenzo[a]xanthen-1 l-ones under solvent-flee conditions.High yields,ease recovery,short reaction time and reusability of catalyst are significant advantages.ZrOCl2·8H2O was also found to act as an effective catalyst towards this transformation.

  10. AgOTf-catalyzed one-pot reactions of 2-alkynylbenzaldoximes with α,β-unsaturated carbonyl compounds

    Directory of Open Access Journals (Sweden)

    Qiuping Ding

    2013-09-01

    Full Text Available AgOTf-catalyzed one-pot reactions of 2-alkynylbenzaldoximes with various α,β-unsaturated carbonyl compounds under mild conditions are described, which provides a facile and efficient pathway for the synthesis of 1-alkylated isoquinoline derivatives. The method tolerates a wide range of substrates and allows for the preparation of the products of interest in moderate to excellent yields.

  11. One-Pot Syntheses of 3, 4-Dihydropyrimidine-2 ( 1H )-thiones Catalyzed by La(OTf)3

    Institute of Scientific and Technical Information of China (English)

    CHEN,Rui-Fang(陈瑞芳); QIAN,Chang-Tao(钱长涛)

    2002-01-01

    A general and practical procedure for the syntheses of 3,4-dihydropyrimidine-2(1H)-thiones by a one-pot condensation of aldehyde, β-ketoester or β-diketone and thiourea using La(OTf)3 as the catalyst is described. Mild reaction conditions,excellent yields as well as the environmentally friendly character ofLa( OTf)3 make it an important alternative to the classic acid-catalyzed Bigineili' s reaction.

  12. One-pot, solvent-free, and efficient synthesis of 2,4,6-triarylpyridines using CoCl2.6H2O as a recyclable catalyst

    Directory of Open Access Journals (Sweden)

    Mahmood Kamali

    2016-12-01

    Full Text Available A one-pot, three components coupling of aryl aldehyde, acetophenone, and ammonium acetate was performed to afford the corresponding 2,4,6-triarylpyridines (TAP1–17. The TAP1–17 were synthesized in the presence of cobalt(II chloride hexahydrate (CoCl2.6H2O via an improved Chichibabin pyridine synthesis protocol. This study has shown that CoCl2.6H2O promotes this reaction in comparison to other transition metal salt such as with FeCl3, NiCl2.6H2O, CuCl2.2H2O, CdCl2.H2O, SbCl3, SnCl2.2H2O, and ZnCl2. This method has several advantages, for example, excellent yields, short reaction times, easy work up, and solvent-free condition. Also, this catalyst was recyclable for four consecutive runs.

  13. Cobalt Nanoparticles Promoted Highly Efficient One Pot Four-Component Synthesis of 1,4-Dihydropyridines under Solvent-Free Conditions%Cobalt Nanoparticles Promoted Highly Efficient One Pot Four-Component Synthesis of1,4-Dihydropyridines under Solvent-Free Conditions

    Institute of Scientific and Technical Information of China (English)

    Javad SAFARI; Sayed Hossein BANITABA; Shiva DEHGHAN KHALILI

    2011-01-01

    A straightforward and general method has been developed for the synthesis of Cs-unsubstitiuted 1,4-dihydropyridines by a reaction using dimedone,acetophenone,aromatic aldehydes,and ammonium acetate in the presence of a catalytic amount of Co nanoparticles as a heterogeneous and eco-friendly catalyst with high catalytic activity at room temperature under solvent-free conditions.This catalyst is easily separated by magnetic devices and can be reused without any apparent loss of activity for the reaction.In addition,it is very interesting that when using Co nanoparticles as a catalyst,spatially-hindered aldehydes such as 2-methoxy-,2-fluoro-,and 2-chloro-aldehydes are suitable for this reaction.

  14. CERIC AMMONIUM NITRATE CATALYZED ONE-POT SYNTHESIS OF NOVEL ISOXAZOLYL-HEXAHYDROQUININDOLINONES Cerammoniumnitrat KATALYSIERTEN ONE-POT Synthese von neuartigen Isoxazolyl-HEXAHYDROQUININDOLINONES

    Directory of Open Access Journals (Sweden)

    E. Rajanarendar, P. Venkateshwarlu, S. Rama Krishna

    2012-07-01

    Full Text Available The ceric ammonium nitrate (CAN catalyzed synthesis of novel isoxazolylhexahydroquinindolinones 4 were simply achieved upon the reaction of isoxazolyl-2-indolinone 1 with 3-amino-5-methyl-isoxazole 2 and dimedone 3 in ethanol with good yields from commercially available materials.

  15. One-pot conversion of disaccharide into 5-hydroxymethylfurfural catalyzed by imidazole ionic liquid.

    Science.gov (United States)

    Qu, Yongshui; Li, Li; Wei, Quanyuan; Huang, Chongpin; Oleskowicz-Popiel, Piotr; Xu, Jian

    2016-01-01

    Conversion of carbohydrate into 5-hydroxymethylfurfural (5- HMF), a versatile, key renewable platform compound is regarded as an important transformation in biomass-derived carbohydrate chemistry. A variety of ILs, not only acidic but also alkaline ILs, were synthesized and used as catalyst in the production of 5-HMF from disaccharide. Several factors including reaction temperature, IL dosage, solvent and reaction time,were found to influence the yield of 5-HMF from cellobiose. Of the ILs tested, hydroxy-functionalized ionic liquid (IL), 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate ([AEMIM]BF4) showed the highest catalytic activity and selectivity. 5-HMF yield of 68.71% from sucrose was obtained after 6 hrs at 160 °C. At the same condition with cellobiose as substrate, 5-HMF yield was 24.73%. In addition, 5-HMF also exhibited good stablity in this reaction system. Moreover, a kinetic analysis was carried out in both acidic and alkaline IL-catalyzed system, suggesting main side reaction in the conversion of fructose catalyzed by acidic and alkaline IL was polymerization of fructose and 5-HMF degradation, respectively. PMID:27181523

  16. 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.

  17. Ferric hydrogensulfate catalyzed synthesis of aryl 14H-dibenzo[a,j] xanthene derivatives under thermal and solvent-free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Shaterian, Hamid Reza; Ghashang, Majid [University of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of). Faculty of Sciences. Dept. of Chemistry]. E-mail: hrshaterian@hamoon.usb.ac.ir

    2008-07-01

    Ferric hydrogensulfate as catalyst has been used for the one-pot preparation of aryl 14Hdibenzo[a,j]xanthene derivatives by cyclocondensation of {beta}-naphthol and substituted benzaldehydes under solvent-free and thermal conditions. This method has the advantages of high yields, a cleaner reaction, simple methodology, short reaction times, easy workup and greener conditions. (author)

  18. 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.

  19. Ferric hydrogensulfate catalyzed aerobic oxidative coupling of 2-naphthols in water or under solvent free conditions

    Institute of Scientific and Technical Information of China (English)

    Hossein Eshghi; Mehdi Bakavoli; Hassanali Moradi

    2009-01-01

    The symmetric oxidative coupling reactions of 2-naphthol derivatives withboth ferric hydrogensulfate in water and silica ferric hydrogensulfate in solvent free conditions were carried out. The advantages of this green procedure are: inexpensive catalyst or co-catalyst, reusability of catalyst, organic solvent-free procedures and simple workup.

  20. Ultrasound assisted enzyme catalyzed hydrolysis of waste cooking oil under solvent free condition.

    Science.gov (United States)

    Waghmare, Govind V; Rathod, Virendra K

    2016-09-01

    The present work demonstrates the hydrolysis of waste cooking oil (WCO) under solvent free condition using commercial available immobilized lipase (Novozyme 435) under the influence of ultrasound irradiation. The process parameters were optimized using a sequence of experimental protocol to evaluate the effects of temperature, molar ratios of substrates, enzyme loading, duty cycle and ultrasound intensity. It has been observed that ultrasound-assisted lipase-catalyzed hydrolysis of WCO would be a promising alternative for conventional methods. A maximum conversion of 75.19% was obtained at mild operating parameters: molar ratio of oil to water (buffer pH 7) 3:1, catalyst loading of 1.25% (w/w), lower ultrasound power 100W (ultrasound intensity - 7356.68Wm(-2)), duty cycle 50% and temperature (50°C) in a relatively short reaction time (2h). The activation energy and thermodynamic study shows that the hydrolysis reaction is more feasible when ultrasound is combined with mechanical agitation as compared with the ultrasound alone and simple conventional stirring technique. Application of ultrasound considerably reduced the reaction time as compared to conventional reaction. The successive use of the catalyst for repetitive cycles under the optimum experimental conditions resulted in a loss of enzymatic activity and also minimized the product conversion. PMID:27150746

  1. Ultrasound assisted enzyme catalyzed hydrolysis of waste cooking oil under solvent free condition.

    Science.gov (United States)

    Waghmare, Govind V; Rathod, Virendra K

    2016-09-01

    The present work demonstrates the hydrolysis of waste cooking oil (WCO) under solvent free condition using commercial available immobilized lipase (Novozyme 435) under the influence of ultrasound irradiation. The process parameters were optimized using a sequence of experimental protocol to evaluate the effects of temperature, molar ratios of substrates, enzyme loading, duty cycle and ultrasound intensity. It has been observed that ultrasound-assisted lipase-catalyzed hydrolysis of WCO would be a promising alternative for conventional methods. A maximum conversion of 75.19% was obtained at mild operating parameters: molar ratio of oil to water (buffer pH 7) 3:1, catalyst loading of 1.25% (w/w), lower ultrasound power 100W (ultrasound intensity - 7356.68Wm(-2)), duty cycle 50% and temperature (50°C) in a relatively short reaction time (2h). The activation energy and thermodynamic study shows that the hydrolysis reaction is more feasible when ultrasound is combined with mechanical agitation as compared with the ultrasound alone and simple conventional stirring technique. Application of ultrasound considerably reduced the reaction time as compared to conventional reaction. The successive use of the catalyst for repetitive cycles under the optimum experimental conditions resulted in a loss of enzymatic activity and also minimized the product conversion.

  2. 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.

  3. Ca(NO3)2·4H2O-catalysed Biginelli Reaction: One-pot Synthesis of 1,2,3,4-Tetrahydropyrimidin-2-ones/pyrimidine-2-thiones under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    DEBACHE Abdelmadjid; BOULCINA Raouf; TAFER Radia; BELFAITAH Ali; RHOUATI Salah; CARBONI Bertrand

    2008-01-01

    The synthesis of 1,2,3,4-dihydropyrimidinone/thione derivatives was achieved in good to excellent yields using calcium(Ⅱ)nitrate as catalyst to promote the Biginelli three-component condensation reaction from a diversity of aromatic aldehydes,β-keto compounds and urea or thiourea.The reaction was carried out under solvent-free condi-tions.

  4. L-Proline Catalyzed Solvent-Free Knoevenagel Condensation for the Synthesis of 3-Substituted Coumarins

    Institute of Scientific and Technical Information of China (English)

    KARADE Nandkishor. N.; GAMPAWAR Sumit V.; SHINDE Sandeep. V.; JADHAV Wamanrao. N.

    2007-01-01

    L-Proline was utilized as an efficient organo-catalyst for the environmentally benign synthesis of 3-substituted coumarins by the Knoevenagel condensation of substituted 2-hydroxybenzaldehydes with reactive methylene compounds under solvent free conditions.

  5. One-Pot Synthesis of 5-Alkoxycarbonyl-4-aryl-3,4-dihydropyrimidin-2- ones Catalyzed by Phosphotungstic Acid

    Institute of Scientific and Technical Information of China (English)

    JIN Tong-Shou; XIAO Jin-Chong; LI Tong-Shuang

    2003-01-01

    @@ Many dihydropyrimidinones and their derivatives play an important role in medicine due to their therapeutic and pharmacological properties. [1] They have emerged as the integral backbones of several calcium channel blockers, antihypertensive agents, alpha-1α-antagonists. [2] Strategies for the synthesis of dihydropyrimidinone nucleus have varied from one-pot to multistep approaches. Although high yields can be achieved by the following complex multistep procedures, these methods lack the simplicity comparing with Biginelli protocol which firstly reported by Biginelli by one-pot condensation of aryl aldehyde, β-ketoesters and urea with catalytic acid in 1993, and these multistep methods suffer from low yields particularly for substituted aromatic aldehyde.

  6. CuI-Catalyzed: One-Pot Synthesis of Diaryl Disulfides from Aryl Halides and Carbon Disulfide

    OpenAIRE

    Mohammad Soleiman-Beigi; Azadeh Izadi

    2013-01-01

    A new application of carbon disulfide in the presence of KF/Al2O3 is reported for the synthesis of organic symmetrical diaryl disulfides. These products were synthesized by one-pot reaction of aryl halides with the in situ generated trithiocarbonate ion in the presence of copper under air atmosphere.

  7. Synthesis of Some New 1,4-Dihydropyridine Derivatives through a Facile One-pot Hantzsch Condensation Catalyzed by Triethylamine

    Institute of Scientific and Technical Information of China (English)

    Ghalem, Wassima; Boulcina, Raouf; Debache, Abdelmadjid

    2012-01-01

    A facile and efficient synthesis of new 1,4-dihydropyridine derivatives was reported via Hantzsch three-com- ponent condensation reaction of aldehydes or formylphenylboronic acids, ethyl acetoacetate, and ammonium acetate in the presence of a catalytic amount of triethylamine under solvent-free conditions. The method described here of- fers several advantages including high yields, short reaction times, and simple work-up procedure.

  8. Ultrasound assisted N-bromosuccinimde catalyzed one pot condensation approach for synthesis of Bis(indolylmethanes from primary alcohols

    Directory of Open Access Journals (Sweden)

    Prakash Chhattise

    2016-07-01

    Full Text Available A simple, efficient protocol for one pot synthesis of bis(indolylmethanes from primary alcohols is investigated with N-bromosuccinimde as a catalyst under ultrasound irradiation. Alcohols can be converted into carbonyl compounds by removal of hydrogen in presence of N-bromosuccinimde as an oxidant and can react in situ with indole to give desired bis(indolylmethanes. In the reported one pot multicomponent condensation reaction N-bromosuccinimde promotes the oxidation of alcohol to aldehyde, facilitating the subsequent condensation with indole to afford bis(indolyl methanes in good to excellent yields. The inexpensiveness and easy handling are some of important feature of N-bromosuccinimde. The by-product N-succinimide can be easily recovered and recycled to N-bromosuccinimide.

  9. One-pot Green Synthesis of Pyrrole Derivatives Catalyzed by Nano Sulfated Zirconia as a Solid Acid Catalyst%One-pot Green Synthesis of Pyrrole Derivatives Catalyzed by Nano Sulfated Zirconia as a Solid Acid Catalyst

    Institute of Scientific and Technical Information of China (English)

    Teimouri, Abbas; Chermahini, Alireza Najafi

    2012-01-01

    A new and efficient method for the preparation of N-substituted pyrroles from one-pot Paal-Knorr condensation has been accomplished using nano-crystalline sulfated zirconia (SZ) as the catalyst in ethanol at moderate temperature. This new protocol has the advantages of easy availability, stability, reusability and eco-friendliness of the catalyst, high to excellent yields, simple experimental and work-up procedure. The synthesized compounds were confirmed through spectral characterization using IR, 1H NMR, 13C NMR and mass spectra.

  10. 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.

  11. L-Proline Catalyzed Enamination of β-Dicarbonyl Compounds under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    KUNDU Dhiman; MAJEE Adinath; HAJRA Alakananda

    2008-01-01

    A simple,general and efficient method has been developed for synthesis of various β-enamino ketones and esters by reacting β-dicarbonyl compounds with amines using a catalytic amount of L-proline at room temperature under solvent-free conditions in excellent yields.

  12. Three-component, one-pot synthesis of benzo[f]indenoquinoline derivatives catalyzed by poly(4-vinylpyridinium) hydrogen sulfate

    Institute of Scientific and Technical Information of China (English)

    Nader Ghaffari Khaligh

    2014-01-01

    7-Aryl-8H-benzo[f]indeno[2,1-b]quinoline-8-one derivatives were synthesized by means of a one-pot condensation of 2-naphthylamine, aromatic aldehydes, and indane-1,3-dione in ethanol under refluxing conditions in the presence of poly(4-vinylpyridinium) hydrogen sulfate, a solid acid catalyst. This method has the advantages of high yield, clean reaction, simple methodology, and short reaction time. The catalyst could be recycled and reused four times without significant loss of activity. The structure of the novel compounds was confirmed by IR, 1H NMR, and 13C NMR spec-troscopy and elemental analysis.

  13. 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.

  14. Solvent-Free Selective Condensations Based on the Formation of the Olefinic (C=C Bond Catalyzed by Organocatalyst

    Directory of Open Access Journals (Sweden)

    Heyuan Song

    2016-07-01

    Full Text Available Pyrrolidine and its derivatives were used to catalyze aldol and Knoevenagel condensations for the formation of the olefinic (C=C bond under solvent-free conditions. The 3-pyrrolidinamine showed high activity and afforded excellent yields of α,β-unsaturated compounds. The aldol condensation of aromatic/heterocyclic aldehydes with ketones affords enones in high conversion (99.5% and selectivity (92.7%. Good to excellent yields of α,β-unsaturated compounds were obtained in the Knoevenagel condensation of aldehydes with methylene-activated substrates.

  15. Asymmetric, Three-Component, One-Pot Synthesis of Spiropyrazolones and 2,5-Chromenediones from Aldol Condensation/NHC-Catalyzed Annulation Reactions.

    Science.gov (United States)

    Wang, Lei; Li, Sun; Chauhan, Pankaj; Hack, Daniel; Philipps, Arne R; Puttreddy, Rakesh; Rissanen, Kari; Raabe, Gerhard; Enders, Dieter

    2016-04-01

    A novel one-pot, three-component diastereo- and enantioselective synthesis of spiropyrazolones has been developed involving the aldol condensation of an enal to generate α,β-unsaturated pyrazolones, which react with a second equivalent of enal through an N-heterocyclic carbene (NHC)-catalyzed [3+2] annulation. The desired spirocyclopentane pyrazolones are obtained in moderate to good yields and good to excellent stereoselectivities. Alternatively, starting from cyclic 1,3-diketones, 2,5-chromenediones are available through [2+4] annulation. PMID:26864437

  16. One-pot, two-step, microwave-assisted palladium-catalyzed conversion of aryl alcohols to aryl fluorides via aryl nonaflates.

    Science.gov (United States)

    Wannberg, Johan; Wallinder, Charlotta; Ünlüsoy, Meltem; Sköld, Christian; Larhed, Mats

    2013-04-19

    A convenient procedure for converting aryl alcohols to aryl fluorides via aryl nonafluorobutylsulfonates (ArONf) is presented. Moderate to good one-pot, two-step yields were achieved by this nonaflation and microwave-assisted, palladium-catalyzed fluorination sequence. The reductive elimination step was investigated by DFT calculations to compare fluorination with chlorination, proving a larger thermodynamic driving force for the aryl fluoride product. Finally, a key aryl fluoride intermediate for the synthesis of a potent HCV NS3 protease inhibitor was smoothly prepared with the novel protocol.

  17. 2-aminopyrimidine-4,6-diol as an efficient ligand for solvent-free copper-catalyzed N-arylations of imidazoles with aryl and heteroaryl halides.

    Science.gov (United States)

    Xie, Ye-Xiang; Pi, Shao-Feng; Wang, Jian; Yin, Du-Lin; Li, Jin-Heng

    2006-10-13

    Efficient and solvent-free copper-catalyzed N-arylations of imidazoles with aryl and heteroaryl halides have been demonstrated. In the presence of CuBr, 2-aminopyrimidine-4,6-diol, and TBAF (n-Bu4NF), a variety of imidazoles underwent the N-arylation reaction with aryl and heteroaryl halides smoothly in moderate to excellent yields. Noteworthy is that the reaction is conducted under solvent-free conditions. PMID:17025338

  18. An Efficient One-pot Synthesis of β-Amino/β-Acetamido Car-bonyl Compounds via ZrCl4-catalyzed Mannich-type Reaction

    Institute of Scientific and Technical Information of China (English)

    SANJEEVA REDDY,Cherkupally; PURNACHANDRA REDDY,Gurrala

    2008-01-01

    Zirconium(IV) chloride catalyzed efficient one-pot synthesis of β-amino/β-acetamido carbonyl compounds at room temperature is described. In the presence of ZrCl4, the three-component Mannich-type reaction via a variety of in situ generated aldimines, with various ketones, aromatic aldehydes and aromatic amines in ethanol, led to the formation of β-amino carbonyl compounds and the four-component Mannich-type reaction of aromatic aldehydes with various ketones, acetonitrile and acetyl chloride resulted in the corresponding β-acetamido carbonyl com-pounds in high to excellent yields. This methodology has also been applied towards the synthesis of dimeric β-amino/β-acetamido carbonyl compounds.

  19. Nickel-Catalyzed Reductive Cross-Coupling of Benzyl Chlorides with Aryl Chlorides/Fluorides: A One-Pot Synthesis of Diarylmethanes.

    Science.gov (United States)

    Zhang, Jie; Lu, Gusheng; Xu, Jin; Sun, Hongmei; Shen, Qi

    2016-06-17

    The first nickel-catalyzed, magnesium-mediated reductive cross-coupling between benzyl chlorides and aryl chlorides or fluorides is reported. A variety of diarylmethanes can be prepared in good to excellent yields in a one-pot manner using easy-to-access mixed PPh3/NHC Ni(II) complexes of Ni(PPh3)(NHC)Br2 (NHC = 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene, IPr, 1a; 1,3-di-tert-butylimidazol-2-ylidene, ItBu, 1b) as catalyst precursors. Activation of polychloroarenes or chemoselective cross-coupling based on the difference in catalytic activity between 1a and 1b is used to construct oligo-diarylmethane motifs. PMID:27268781

  20. Solvent-Free Lipase-Catalyzed Synthesis of Diacylgycerols as Low-Calorie Food Ingredients

    Science.gov (United States)

    Vázquez, Luis; González, Noemí; Reglero, Guillermo; Torres, Carlos

    2016-01-01

    Problems derived from obesity and overweight have recently promoted the development of fat substitutes and other low-calorie foods. On the one hand, fats with short- and medium-chain fatty acids are a source of quick energy, easily hydrolyzable and hardly stored as fat. Furthermore, 1,3-diacylglycerols are not hydrolyzed to 2-monoacylglycerols in the gastrointestinal tract, reducing the formation of chylomicron and lowers the serum level of triacylglycerols by decreasing its resynthesis in the enterocyte. In this work, these two effects were combined to synthesize short- and medium-chain 1,3-diacylglycerols, leading to a product with great potential as for their low-calorie properties. Lipase-catalyzed transesterification reactions were performed between short- and medium-chain fatty acid ethyl esters and glycerol. Different variables were investigated, such as the type of biocatalyst, the molar ratio FAEE:glycerol, the adsorption of glycerol on silica gel, or the addition of lecithin. Best reaction conditions were evaluated considering the percentage of 1,3-DAG produced and the reaction rate. Except Novozym 435 (Candida antarctica), other lipases required the adsorption of glycerol on silica gel to form acylglycerols. Lipases that gave the best results with adsorption were Novozym 435 and Lipozyme RM IM (Rhizomucor miehei) with 52 and 60.7% DAG at 32 h, respectively. Because of its specificity for sn-1 and sn-3 positions, lipases leading to a higher proportion of 1,3-DAG vs. 1,2-DAG were Lipozyme RM IM (39.8 and 20.9%, respectively) and Lipase PLG (Alcaligenes sp.) (35.9 and 19.3%, respectively). By adding 1% (w/w) of lecithin to the reaction with Novozym 435 and raw glycerol, the reaction rate was considerably increased from 41.7 to 52.8% DAG at 24 h. PMID:26904539

  1. Expeditious and Efficient Synthesis of Benzoxazoles, Benzothiazoles, Benzimidazoles Catalyzed by Ga(OTf)3 under Solvent-Free Conditions%Expeditious and Efficient Synthesis of Benzoxazoles, Benzothiazoles, Benzimidazoles Catalyzed by Ga(OTf)3 under Solvent-Free Conditions

    Institute of Scientific and Technical Information of China (English)

    刘巨艳; 刘倩; 徐玮; 王玮璐

    2011-01-01

    A new and efficient method for the synthesis of benzoxazoles, benzothiazoles, benzimidazoles from reactions of o-substituted aminoaromatics with orthoesters in the presence of catalytic amounts of Ga(OTf)3 under solvent-free conditions is presented. The remarkable features of this new protocol are high conversion, very short reaction times, cleaner reaction profiles under solvent-free conditions, straight forward procedure, and use of relatively non-toxic catalysts.

  2. [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.

  3. Regioselective Synthesis of Z-Aldoximes Catalyzed By H3PMo12O40 under Solvent-Free Conditions

    International Nuclear Information System (INIS)

    A facile and efficient method for the preparation of Z-aldoximes is improved by means of H3PMo12O40 catalyst in solvent-free media. The major advantages of this method are: operational simplicity, low catalyst loading, selectivity, mild reaction conditions, short reaction times and excellent yields. The recovered catalyst could be used in new attempts without any purification

  4. B(C6F5)3 catalyzed one-pot three-component Biginelli reaction: An efficient and environmentally benign protocol for the synthesis of 3,4-dihydropyrimidin-2(1)-ones/thiones

    Indian Academy of Sciences (India)

    Santosh Kumar Prajapti; Keshav Kumar Gupta; Bathini Nagendra Babu

    2015-06-01

    Tris(pentafluorophenyl)borane catalyzed, one-pot, simple, efficient and environmentally benign protocol for the synthesis of dihydropyrimidinones/thiones via Biginelli reaction has been described. The main highlights of the present protocol is low catalyst loading, low toxicity, compatibility with acid-labile-protecting groups, short reaction time, consistently excellent yields and simple reaction/workup procedure. Moreover, the applicability of the present methodology for large-scale synthesis of monastrol highlights its potential for bulk synthesis.

  5. A mild and highly efficient one-pot three-component reaction for carbon-sulfur bond formation catalyzed by potassium tert-butoxide

    Institute of Scientific and Technical Information of China (English)

    Barahman Movassagh; Amir Rakhshani

    2011-01-01

    Potassium tert-butoxide has been found to be a highly efficient catalyst for one-pot, three-component reaction of aryl aldehydes, acetophenones, and thiols via Claisen-Schmidt/Michael addition reactions for the synthesis of thia-Michael adducts in high yields. The reactions are best carried out in tert-butyl alcohol at room temperature.

  6. Synthesis of β-arylated alkylamides via Pd-catalyzed one-pot installation of a directing group and C(sp3)–H arylation

    Science.gov (United States)

    Zhang, Yi; Cao, Xiaoji; Wan, Jie-Ping

    2016-01-01

    Summary The synthesis of β-arylated alkylamides via alkyl C–H bond arylation has been realized by means of direct one-pot reactions of acyl chlorides, aryl iodides and 8-aminoquinoline. Depending on the structure of the starting materials, both single and double β-arylated alkylamides could be accessed. PMID:27340500

  7. Phosphotungstic Acid Catalyzed One-Pot Synthesis of 2-amino-3,5-dicarbonitrile-6-thio-pyridines in Aqueous Media

    International Nuclear Information System (INIS)

    In this study, we report the one-pot synthesis of 2-amino-3,5-dicarbonitrile-6-thio-pyridines with benzaldehyde, malononitrile, and thiophenol by using phosphotungstic acid as an efficient catalyst to aqueous media. This method has the advantages of easy separation, high storage stability, and environmental friendliness. (author)

  8. Efficient Synthesis of Pyrrolo[2,1-a]isoquinoline and Pyrrolo[1,2-a]quinoline Derivatives via One-pot Two- step Metal-catalyzed Three-component Reactions

    Institute of Scientific and Technical Information of China (English)

    吴磊; 孙晶; 颜朝国

    2012-01-01

    A sequential one-pot two-step reaction for efficient synthesis of pyrrolo[2,1-a]isoquinoline and pyrrolo[1,2-a]- quinoline derivatives in good yields has been successfully developed. The reaction included firstly Cu-catalyzed three-component reaction of isoquinoline (quinoline), acetylenedicarboxylate and alkynylbenzene and then Pd-catalyzed intramolecular C(sp)-C(sp^2) coupling reaction of initially formed 1-alkenyl-2-alkynyl- 1,2-dihydroiso- quinoline (1,2-dihydroquinoline).

  9. PPA-SiO2 catalyzed efficient synthesis of polyhydroquinoline derivatives through Hantzsch multicomponent condensation under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Amir Khojastehnezhad; Farid Moeinpour; Abolghasem Davoodnia

    2011-01-01

    Silica gel-supported polyphosphoric acid (PPA-SiO2) was found to be an efficient catalyst for the one-pot four-component Hantzsch condensation reaction of aryl aldehydes, dimedone, ethyl acetoacetate and ammonium acetate to afford the corresponding polyhydroquinoline derivatives in high yields. The main advantages of the present approach are short reaction times, clean reaction profiles, simple experimental and workup procedures.

  10. 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

  11. One-Pot Four-Component Dakin-West Synthesis of β-Acetamido Ketones Catalyzed by a Vanadium-Substituted Heteropolyacid

    Institute of Scientific and Technical Information of China (English)

    Reza TAYEBEE; Shima TIZABI

    2012-01-01

    The multicomponent condensation of an aryl aldehyde,acetyl chloride,acetonitrile,and enolizable ketone as one-pot synthesis of β-acetamido ketones in high yields was investigated using commercial,non-corrosive,and environmentally benign Keggin and Wells-Dawson heteropolyacid catalysts.The best catalyst was H5PW10V2O40.The methodology used simple experimental conditions,and the short reaction times and high yields indicate it is a useful strategy for the large scale synthesis of β-acetamido ketones.

  12. 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.

  13. Vanadium Hydrogen Sulfate Catalyzed Solvent-Free Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones and Bis-(indolyl) methanes

    International Nuclear Information System (INIS)

    We have developed a mild, simple and efficient method for the synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones and bis-(indolyl) methanes catalyzed by V(HSO4)3. Based on our studies, this method offers several adavantages including mild reaction conditions, good to high yields of the products, short reaction times, solvent-free reaction conditions and simple experimental procedure. 3,4-Dihydropyrimidin-2(1H)-ones and their derivatives have attracted increasing interest due to their wide range of therapeutical and pharmacological properties, such as antiviral, antitumor, antibacterial, and antiinflammatory properties. Some of them have been successfully used as calcium channel blockers, antihypertensive agents, and α1a-antagonists. Moreover, several marine alkaloids whose molecular structures contain the dihydropyrimidinone core also exhibit interesting biological activities. Therefore, synthesis of these type of compounds is still of great importance

  14. Efficient synthesis of spironaphthopyrano [2,3-d]pyrimidine-5,3'-indolines under solvent-free conditions catalyzed by SBA-Pr-SO3H as a nanoporous acid catalyst.

    Science.gov (United States)

    Ziarani, Ghodsi Mohammadi; Lashgari, Negar; Faramarzi, Sakineh; Badiei, Alireza

    2014-01-01

    A green, simple one-pot synthesis of spironaphthopyrano[2,3-d]pyrimidine-5,3'-indoline derivatives by a three-component reaction of isatins, 2-naphthol, and barbituric acids under solvent-free conditions in the presence of SBA-Pr-SO(3)H has been accomplished. Sulfonic acid functionalized SBA-15 (SBA-Pr-SO(3)H) as a heterogeneous nanoporous solid acid catalyst was found to be an efficient and recyclable acid catalyst in this synthesis. PMID:25286212

  15. One-Pot Synthesis of Pyrrolo[1,2-a]quinoxaline Derivatives via a Copper-Catalyzed Aerobic Oxidative Domino Reaction.

    Science.gov (United States)

    Liu, Huanhuan; Duan, Tiantian; Zhang, Zeyuan; Xie, Caixia; Ma, Chen

    2015-06-19

    A copper-catalyzed process for the synthesis of pyrrolo[1,2-a]quinoxalines from readily available α-amino acids and 1-(2-halophenyl)-1H-pyrroles is described. Different functional groups were well tolerated to give the corresponding products.

  16. Cu(OAc)2/Pyrimidines-Catalyzed Cross-coupling Reactions of Aryl Iodides and Activated Aryl Bromides with Alkynes under Aerobic, Solvent-free and Palladium-free Conditions

    Institute of Scientific and Technical Information of China (English)

    XIE Ye-Xiang; DENG Chen-Liang; PI Shao-Feng; LI Jin-Heng; YIN Du-Lin

    2006-01-01

    Excellent results have been achieved in the Cu(OAc)2-catalyzed Sonogashira cross-couplings of aryl iodides and activated aryl bromides utilizing TBAF (tetrabutylammonium fluoride) as the base and 4,6-dimethoxypyrimidin-2-amine as the ligand. It is noteworthy that the reaction is conducted under aerobic, solvent-free and palladium-free conditions.

  17. 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

  18. 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.

  19. 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.

  20. Highly Efficient and Recyclable Catalyst HBF4·SiO2 Catalyzed Synthesis of β-Enamino Compounds Under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    GAO Han; JIA Xu-dong; DUAN Hai-feng; LIN Ying-jie; GAO Jun-gang; LIANG Da-peng; WU Mao-cheng

    2011-01-01

    Fluoroboric acid adsorbed on silica-gel(HBF4.SiO2) has been found to be an extremely efficient and recyclable catalyst for the preparation ofβ-enaminones and β-enamino esters under solvent-free conditions.

  1. Solvent-free one-pot 1,3-dipolar cycloaddition reactions of dihydropyran derived nitrone

    Indian Academy of Sciences (India)

    Bhaskar Chakraborty; Prawin Kumar Sharma; Neelam Rai; Chiran Devi Sharma

    2012-05-01

    Microwave-induced 1,3-dipolar cycloaddition reactions of dihydropyran derived nitrone with various activated alkenes have been studied in situ and found to afford new isoxazolidine derivatives with moderate selectivity.

  2. 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.

  3. New Efficient Synthesis of 3,4-Dihydropyrimidin-2(1H-ones Catalyzed by Benzotriazolium-Based Ionic Liquids under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Zhiqing Liu

    2016-04-01

    Full Text Available An efficient synthesis of novel 3,4-dihydropyrimidin-2(1H-ones (DHPMs and their derivatives, using Brønsted acidic ionic liquid [C2O2BBTA][TFA] as a catalyst, from the condensation of aryl aldehyde, β-ketoester and urea was described. Reactions proceeded smoothly for 40 min under solvent-free conditions and gave the desirable products with good to excellent yields (up to 99%. The catalyst could be easily recycled and reused with similar efficacies for at least six cycles.

  4. New Efficient Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones Catalyzed by Benzotriazolium-Based Ionic Liquids under Solvent-Free Conditions.

    Science.gov (United States)

    Liu, Zhiqing; Ma, Rong; Cao, Dawei; Liu, Chenjiang

    2016-01-01

    An efficient synthesis of novel 3,4-dihydropyrimidin-2(1H)-ones (DHPMs) and their derivatives, using Brønsted acidic ionic liquid [C₂O₂BBTA][TFA] as a catalyst, from the condensation of aryl aldehyde, β-ketoester and urea was described. Reactions proceeded smoothly for 40 min under solvent-free conditions and gave the desirable products with good to excellent yields (up to 99%). The catalyst could be easily recycled and reused with similar efficacies for at least six cycles. PMID:27070558

  5. Cu-doped ZnO nanocrystalline powder catalyzed one-pot synthesis of fully substituted new indeno[1,2-b]pyridines at room temperature by a multi-component reaction

    Institute of Scientific and Technical Information of China (English)

    Heshmatollah Alinezhad; Sahar Mohseni Tavakkoli; Pourya Biparva

    2014-01-01

    Cu doped ZnO nanocrystalline powder (10 mol%) has been found to be an efficient catalyst for the one-pot multi-component synthesis of fully substituted new indeno[1,2-b]pyridines through a com-bination of 1,3-indandione, propiophenone or acetophenone derivatives, aromatic aldehydes, and ammonium acetate in ethanol/H2O at room temperature. The methodology is mild, efficient and high to excellent yielding.

  6. Alum:An efficient catalyst for one-pot synthesis of a-aminophosphonates

    Institute of Scientific and Technical Information of China (English)

    Swapnil S.Sonar; Kiran F.Shelke; Gopal K.Kakade; Bapurao B.Shingate; Murlidhar S.Shingare

    2009-01-01

    Alum(KA1(SO4)2·12H2O)is an inexpensive,efficient,non-toxic and mild catalyst for the one-pot synthesis of a-aminophosphonates.A three component reaction of an aldehyde/ketone,an amine and triethyl phosphite was carried out under solvent-free conditions to afford the corresponding a-aminophosphonates in short reaction times and high yields with the green aspects by avoiding toxic catalysts and solvents.

  7. ZrOC12·8H2O catalyzed one-pot synthesis of 2,4,5-triaryl-1H-imidazoles and substituted 1,4-di(4,5-diphenylimidazolyl)benzene

    Institute of Scientific and Technical Information of China (English)

    Jaiprakash N.Sangshetti; Nagnnath D.Kokare; Sandeep A.Kotharkar; Devanand B.Shinde

    2008-01-01

    A simple one-pot synthetic method for the preparation of 2,4,5-triaryl-lH-imidazoles from benzoin or benzil,ammonium acetate,aromatic aldehydes,and ZrOCl 2·8H 2O catalyst is described.The ZrOCl2-8H2O catalyst was found to be equally effective for aromatic and heteroaromatic aldehydes and also for the preparation of substituted 1,4-di(4,5-diphenylimidazol-yl) benzene.

  8. Zeolite H-BEA catalysed multicomponent reaction: One-pot synthesis of amidoalkyl naphthols - Biologically active drug-like molecules

    Indian Academy of Sciences (India)

    Sunil R Mistry; Rikesh S Joshi; Kalpana C Maheria

    2011-07-01

    Zeolite has been used as an efficient and a novel heterogeneous catalyst for one-pot synthesis of biologically active drug-like molecules, amidoalkyl naphthols. This green route involves multicomponent reaction of 2-naphthol, aromatic aldehydes and amide in the presence of a catalytic amount of zeolite H-Beta (H-BEA) under solvent reflux as well as solvent-free conditions.

  9. Water mediated eco-friendly green protocol for one-pot synthesis of -aminophosphonates at ambient conditions

    Indian Academy of Sciences (India)

    Santhosh Reddy Mandha; Manjula Alla; Vittal Rao Bommena

    2014-05-01

    Increasing environmental awareness and economic concerns have led to the consideration of highly efficient one-pot, three-component, green approaches for important organic synthons. We describe here a simple, elegant and high yielding protocol for the synthesis of -aminophosphonates in totally solvent-free, catalyst-free conditions by reacting aldehydes, amines and trimethyl phosphite at ambient temperature.

  10. Enzymatically catalyzed synthesis of anti-blooming agent 1,3-dibehenoyl-2-oleoyl glycerol in a solvent-free system: optimization by response surface methodology.

    Science.gov (United States)

    Meng, Zong; Geng, Wen-Xin; Li, Jin-Wei; Yang, Zhao-Qi; Jiang, Jiang; Wang, Xing-Guo; Liu, Yuan-Fa

    2013-11-13

    Products rich in 1,3-dibehenoyl-2-oleoyl glycerol (BOB) triglyceride (TAG) were produced by enzymatic interesterification of high oleic acid sunflower oil (HOSO) and behenic acid methyl ester (BME) by 1,3-regiospecific lipase Lipozyme RM IM in a solvent-free system. The impact factors of enzyme load, substrate molar ratio of BME to HOSO (BME/HOSO), reaction time, reaction temperature, and pre-equilibration water activity of the enzyme on BOB content and BME conversions were investigated by single-factor experiments and then optimized using the response surface methodology (RSM). The optimum conditions were as follows: reaction temperature, 72 °C; reaction time, 7.99 h; substrate molar ratio, 2.5:1; enzyme load, 10%; and pre-equilibration water activities of the enzyme, 0.28. The results from the experiments conducted according to the predicted optimal conditions were as follows: the content of BOB was 32.76%, and the conversion of BME was 65.16%. The experimental values agreed with the predicted values, which verified the sufficiency of the quadratic regression models. After purification under the optimal short-range molecular distillation and two-step solvent fractionation, the content of BOB in the target product can reach 77.14%, indicating the great potential for industrial production of the anti-blooming agent. PMID:24147905

  11. 响应面法优化无溶剂体系酶法合成己酸乙酯%Optimization of Lipase-Catalyzed Synthesis of Ethyl Hexanoate in Solvent Free System by Response Surface Methodology

    Institute of Scientific and Technical Information of China (English)

    赵磊; 程玥; 王成涛

    2012-01-01

    目的:探讨无溶剂体系酶法合成己酸乙酯的最佳工艺条件。方法:在单因素试验的基础上,以脂肪酶添加量、底物(己酸/乙醇)物质的量比、反应时间为影响因素,应用二次回归中心组合试验法进行三因素五水平试验,以己酸乙酯产率为评价指标,进行响应面分析。结果:无溶剂体系酶法合成己酸乙酯的最佳工艺条件为脂肪酶添加量0.5%、酸醇物质的量比1:1.3、反应时间12.2h、反应温度30℃,转速150r/min。在此条件下,己酸乙酯产率实际值为81.6%,与预测值相近。结论:采用中心组合试验设计——响应面法对无溶剂体系酶法合成己酸乙酯工艺条件进行优化合理可行。%Objective: To optimize lipase-catalyzed synthesis of ethyl hexanoate in a solvent-free system. Methods: One-factor- at-a-time experiments were cairred out to identify lipase amount, molar ratio of hexanoic acid to ethanol and reaction time as main variables that influence ethyl hexanoate yield for response surface optimization based on a three-valrable, five-level central composite design. Results: The optimum conditions for lipase-catalyzed synthesis of ethyl hexanoate were determined as 0.5% of enzyme amount, 1:1.3 of molar ratio of hexanoic acid to ethanol, 12.2 h of reaction time and 30 ℃ of reaction temperature, and 150 r/min of rotary speed. Under these conditions, the experimental value of ethyl bexanoate yield was 81.6%, which was close to the predicted value (87.7%). Conclusion: It is feasible to optimize lipase-catalyzed synthesis of ethyl hexanoate in a solvent- free system by response surface methodology.

  12. One-pot synthesis of arene-fused 2-acylcyclohexenones from propargylic carboxylates

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    From readily available propargylic carboxylates, two sequential transformations―gold-catalyzed tandem reactions and Sc(OTf)3-catalyzed cyclization―in a one-pot process led to the formation of 2-acylcyclohexenones with an electron-rich arene ring fused at the 4,5-positions.

  13. One-pot synthesis of arene-fused 2-acylcyclohexenones from propargylic carboxylates

    Institute of Scientific and Technical Information of China (English)

    CAO SanSan; ZHANG LiMing

    2009-01-01

    From readily available propargylic carboxylates,two sequential transformations-gold-catalyzed tandem reactions and ScOTf3-catalyzed cyclization-in a one-pot process led to the formation of 2-acylcyclohexenones with an electron-rich arene ring fused at the 4,5-positions.

  14. Solar thermochemical reactions Ⅲ: A convenient one-pot synthesis of 1,2,4,5-tetrasubstituted imidazoles catalyzed by high surface area SiO2 and induced by solar thermal energy

    Institute of Scientific and Technical Information of China (English)

    Ramadan A. Mekheimer; Afaf M. Abdel Hameed; Seham A.A. Mansour; Kamal Usef Sadek

    2009-01-01

    A simple, convenient and efficient method for the synthesis of 1,2,4,5-tetrasubstituted imidazole derivatives using benzoin, an aromatic aldehyde, an aromatic amine in the presence of ammonium acetate catalyzed by high surface area SiO2 and induced by free solar thermal energy was reported.

  15. 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

    2014-01-01

    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.

  16. TBAHS CATALYZED COUPLING REACTIONS OF ARYL IODIDES AND ARYL BROMIDES WITH THIOLS UNDER SOLVENT FREE CONDITIONS TBAHS katalysierten Kupplungen von Aryliodiden und-Arylbromiden mit Thiolen unter lösungsmittelfreien freien Bedingungen

    Directory of Open Access Journals (Sweden)

    Gajendera Singha, Ajay kumarb , Sakshi Malikc, Preeti Chaudharyd

    2013-04-01

    Full Text Available A recyclable and efficient Tetrabutylammonium hydrogensulfate (TBAHS catalysed coupling reaction of aryl halides (iodide and bromide with aryl and alkyl thiols under solvent-free conditions were developed.

  17. One-pot efficient green synthesis of 1,4-dihydro-quinoxaline-2,3-dione derivatives

    Indian Academy of Sciences (India)

    Harjyoti Thakuria; Gopal Das

    2006-09-01

    An efficient synthesis of the potential pharmacophore 1,4-dihydro-quinoxaline-2,3-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 X-ray diffraction analysis was carried out for some hydrated crystals.

  18. One-pot three-component Biginelli-type reaction to synthesize 3,4-dihydropyrimidine-2-(1H)-ones catalyzed by Co phthalocyanines: Synthesis, characterization, aggregation behavior and antibacterial activity.

    Science.gov (United States)

    Medyouni, Rawdha; Elgabsi, Wissal; Naouali, Olfa; Romerosa, Antonio; Sulaiman Al-Ayed, Abdullah; Baklouti, Lasaad; Hamdi, Naceur

    2016-10-01

    The synthesis of a novel phthalonitrile derivative with pyridine-2-thiol and 2,4,6-trimethylphenylamine substituents functionalized groups and its peripherally tetrasubstituted cobalt phthalocyanine and cationic phthalocyanines complexes were reported. The aggregation investigations carried out in different concentrations indicate that Co Phthalocyanines compounds 3,4 do not have any aggregation behavior for the concentration range of 6×10(-4)-14×10(-6)M in DMSO. The ion binding properties of Co Phthalocyanines compounds 3,4 show the formation of stable complex with Co(2+). In addition 3,4-Dihydropyrimidin-2(1H)-one derivatives were synthesized by modified Biginelli cyclocondensation reaction catalyzed by MPc as Lewis base. The structures of the synthesized compounds have been successfully characterized by the spectroscopic methods (IR, (1)H NMR, (13C)NMR, UV-Vis, mass spectrometry, elemental analysis and NMR 2D). The influence of substrate/catalyst ratio, solvent was also investigated to find optimal reaction on this synthesis for getting the highest conversion. Different parameters were examined for finding optimal conditions of catalysis. In addition; the compounds 3-11 were investigated for antimicrobial activity. Most of them exhibited important antimicrobial activity. PMID:27287623

  19. Bis(imino)pyridine (BIMP) Fe(II) catalyses one-pot green condensation of resorcinol, malononitrile, aromatic aldehydes and cyclohexanone

    Indian Academy of Sciences (India)

    Saman Damavandi; Reza Sandaroos

    2012-03-01

    A novel, efficient and green approach for the synthesis of pyranopyridine derivatives through one-pot, four-component reaction of resorcinol, malononitrile, aromatic aldehydes and cyclohexanone using bis(imino)pyridine (BIMP) Fe(II) catalyst under solvent-free and ultrasonic irradiation is described.

  20. Nano-sulfated zirconia as an efficient, recyclable and environmentally benign catalyst for one-pot three component synthesis of amidoalkyl naphthols

    Institute of Scientific and Technical Information of China (English)

    Abbas Zali; Arash Shokrolahi

    2012-01-01

    One pot synthesis of amidoalkyl naphthols by reaction of aromatic aldehydes,2-naphthol and amide/urea using nano-sulfated zirconia as a catalyst is reported.The reaction was carried out under solvent-free conditions.The method gave good yields of amidoalkyl naphthols in short reaction time.The catalyst is recycled for five consecutive times without loss of activity.

  1. An environmentally benign three component one-pot synthesis of amidoalkyl naphthols using H4SiW12O40 as a recyclable catalyst

    Indian Academy of Sciences (India)

    Amit R Supale; Gavisiddappa S Gokavi

    2010-03-01

    One pot synthesis of amidoalkyl naphthol by condensation of aromatic aldehydes, 2-naphthol and amide/urea using silicotungstic acid as a catalyst is reported. The reaction was carried out under solvent-free reaction conditions. The method gave good yields of amidoalkyl naphthols in short reaction time compared with previous methods. The catalyst is recycled for five consecutive times without loss of activity.

  2. One-pot peptide and protein conjugation: a combination of enzymatic transamidation and click chemistry.

    Science.gov (United States)

    Rachel, N M; Pelletier, J N

    2016-02-11

    Enzymatic transamidation and copper-catalyzed azide-alkyne cycloaddition (CuAAC) were combined to yield covalently conjugated peptides and proteins. The addition of glutathione preserved enzymatic activity in the presence of copper. Tuning the reaction kinetics was key to success, providing up to 95% conversion. This one-pot reaction allowed for targeted fluorescent protein labeling. PMID:26741126

  3. The use of calcium carbide in one-pot synthesis of symmetric diaryl ethynes.

    Science.gov (United States)

    Zhang, Weiwei; Wu, Huayue; Liu, Zhiqing; Zhong, Ping; Zhang, Lin; Huang, Xiaobo; Cheng, Jiang

    2006-12-14

    An efficient Pd-catalyzed copper and amine free coupling reaction of acetylene and aryl bromides was achieved with calcium carbide as an acetylene source, using inorganic base and easily prepared, air-stable aminophosphine ligand in common organic solvents, providing symmetric diaryl ethynes in one-pot with yields ranged from moderate to excellent.

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

    Science.gov (United States)

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

    2016-05-01

    A new oxime-imine functionalized highly ordered mesoporous SBA-15 (SBA-15-NH2-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(ClO4)2 to yield the functionalized nickel catalyst SBA-15-NH2-DAMO-Ni. All the synthesized materials were thoroughly characterized using different characterization techniques. It was found that SBA-15-NH2-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.

  5. Microwave-assisted solvent-free synthesis of 14-aryl/alkyl-14H-dibenzo[a,j]xanthenes and tetrahydrobenzo[a]xanthen-11-ones catalyzed by nano silica phosphoric acid

    OpenAIRE

    Abdolhamid Bamoniri; Bi Bi Fatemeh Mirjalili; Sedigeh Nazemian

    2013-01-01

    Nano silica phosphoric acid (nano SPA) was applied as a catalyst for synthesis of 14-aryl/alkyl-14H-dibenzo[a,j]xanthenes and tetrahydrobenzo[a]xanthen-11-ones in microwave oven under solvent free conditions. High efficiency, easy availability and reusability are some advantages of this catalyst.

  6. One pot synthesis of bis-silicon-bridged stilbene derivatives

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Bis-silicon-bridged stilbene derivatives were synthesized in a modified procedure that combined the preparation of bis[2-(silyl)phenyl]acetylene and its intrmolecular reductive cyclization in one pot. The results indicated that the one pot approach produced target products in a comparable yield to that of the two-step method reported previously.

  7. One-pot synthesis of tetrazole-1,2,5,6-tetrahydronicotinonitriles and cholinesterase inhibition: Probing the plausible reaction mechanism via computational studies.

    Science.gov (United States)

    Hameed, Abdul; Zehra, Syeda Tazeen; Abbas, Saba; Nisa, Riffat Un; Mahmood, Tariq; Ayub, Khurshid; Al-Rashida, Mariya; Bajorath, Jürgen; Khan, Khalid Mohammed; Iqbal, Jamshed

    2016-04-01

    In the present study, one-pot synthesis of 1H-tetrazole linked 1,2,5,6-tetrahydronicotinonitriles under solvent-free conditions have been carried out in the presence of tetra-n-butyl ammonium fluoride trihydrated (TBAF) as catalyst and solvent. Computational studies have been conducted to elaborate two plausible mechanistic pathways of this one-pot reaction. Moreover, the synthesized compounds were screened for cholinesterases (acetylcholinesterase and butyrylcholinesterase) inhibition which are consider to be major malefactors of Alzheimer's disease (AD) to find lead compounds for further research in AD therapy.

  8. One-pot synthesis and UV-Visible absorption studies of novel tricyclic heterocycle tethered Xanthene-1,8-diones

    Indian Academy of Sciences (India)

    Thirumal Yempala; Balasubramanian Sridhar; Srinivas Kantevari

    2015-05-01

    A series of new tricyclic heterocyclic xanthene-1,8-diones tethered with chromophoric dibenzo [ , ]furan, dibenzo[ , ]thiophene and 9-methyl-9-carbazoles were synthesized through one-pot condensation of dibenzo[ , ]furan-2-carbaldehyde, dibenzo[ , ] thiophene-2-carbaldehyde and 9-methyl-9-carbazole-3-carbaldehyde with cyclic 1,3-dicarbonyls in the presence of recyclable PPA-SiOM2 catalyst under solvent-free conditions. Further, UV-Visible absorption properties of all the synthesized compounds were investigated in CHCl3, THF and acetonitrile.

  9. 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.

  10. Solvent-Free Synthesis of New Coumarins

    Directory of Open Access Journals (Sweden)

    Redah I. Al-Bayati

    2012-01-01

    Full Text Available A solvent-free synthesis of five series of coumarin derivatives using microwave assistant is presented herein. The synthesized compounds are fully characterized by UV-VIS, FT-IR, and NMR spectroscopy.

  11. 无溶剂条件下碱性离子液体催化查尔酮的绿色化合成%A Green Synthesis of Chalcones Catalyzed by An Alkaline Ionic Liquid under Solvent-Free Condition

    Institute of Scientific and Technical Information of China (English)

    胡晓允; 韦丽艳; 钟诗施; 谢金生

    2015-01-01

    在无溶剂条件下,将碱性离子液体—乙醇胺乙酸盐用于催化苯乙酮与醛的Claisen-Schmidt 缩合反应制备了查尔酮。结果表明:该碱性离子液体表现出良好的催化活性和循环催化性能。%An alkaline ionic liquid—2-hydroxyethyl ammonium acetate was used as catalyst for Claisen-Schmidt condensation between acetophenone and aromatic aldehydes to prepare chalcones under solvent-free condition. The results indicated that this alkaline ionic liquid showed good catalytic activity and recyclability.

  12. New observation on a class of old reactions:Chemoselectivity for the solvent-free reaction of aromatic aldehydes with alkylketones catalyzed by a double-component inorganic base system

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Solvent-free reactions of aromatic aldehydes with three representative ketones,including acetophenone,acetone and cyclohexanone,have been examined under the catalysis of a low-cost inorganic base system consisting of NaOH and K2CO3.It was found that the chemoselectivity of the reactions is in close relationship with the composition of the reactants and the doublecomponent catalyst.Under the optimized experimental conditions,1,2,3,4,5-pentasubstituted cyclohexanols,α,β-unsaturated ketones and Claisen-Schmidt bicondensation products were obtained in high yields.Two Kostanecki’s triketones were separated,The composition and structure were affirmed by X-ray crystallographic analysis.

  13. Fluorine-18 labeling by click chemistry: Multiple probes in one pot

    International Nuclear Information System (INIS)

    Click chemistry has been widely applied in drug development including radiopharmaceuticals and has shown great advantages. Here we reported a novel strategy for rapid preparation of multiple 18F labeled PET probes in one pot using the ‘Click Reaction’ of Cu(I)-catalyzed Huisgen 1,3-dipolar cycloaddition of terminal alkynes and organic azides (CuAAC). Preliminary results showed its high efficiency and potential for speeding up the preclinical screening of PET probes. - Highlights: ► With click labeling method, multiple PET probes can be labeled in one pot with high efficiency. ► Under proper HPLC conditions, multiple probes can be separated with high radiochemical purities and chemical purities. ► This strategy if combined with high throughout screening, the discovery of PET probes may be accelerated

  14. Efficient Solvent-free Synthesis of Chloropropene Carbonate from the Coupling Reaction of CO2 and Epichlorohydrin Catalyzed by Magnesium Porphyrins as Chlorophyll-like Catalysts%类叶绿素镁卟啉高效催化CO2环氧氯丙烷偶合反应无溶剂合成氯丙烯碳酸酯

    Institute of Scientific and Technical Information of China (English)

    王梅; 佘远斌; 周贤太; 纪红兵

    2011-01-01

    Highly efficient solvent-free coupling reaction of carbon dioxide (CO2) and epichlorohydrin catalyzed by meso-tetraphenyl porphyrin magnesium (MgTPP) in the presence of triethylamine as co-catalysts is reported. As a chlorophyll-like catalyst, MgTPP showed excellent activity for the coupling reaction of CO2 and epichlorohydrin to chloropropene carbonate, in which the turnover number could reach up to 9200. Moreover, different factors including the amount of catalyst, reaction temperature, pressure and time were systematically investigated and the optimal reaction conditions were obtained (epichlorohydrin 50 mmol, MgTPP 5.0×10-3 mmol, triethylamine 6.25x10-3 mmol, 140 ℃, 1.5 MPa, 8 h). A plausible two-pathway mechanism for the coupling reaction of CO2 and epichlorohydrin is proposed to propound the catalysis of MgTPP.

  15. A One-pot Green Synthesis of Alkylidenesuccinimides

    Institute of Scientific and Technical Information of China (English)

    Yan, Lin; Yang, Wenguo; Li, Lixin; Shen, Yang; Jiang, Zhiyong

    2011-01-01

    A mild and facile Wittig reaction between N-substituted maleimides and aldehydes has been developed. Various synthetically valuable alkylidenesuccinimides were obtained from this one-pot reaction in high yields (up to 99%). The product was obtained by simple filtration and no extra purification was necessary. Ethanol, an environment-benign solvent, was found to be a suitable reaction medium.

  16. A One-pot Procedure to Prepare Ethynylferrocene and Iodoethynylferrocene

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Ethynylferrocene and iodoethynylferrocene were prepared in high yield as 88-90% through a one-pot procedure.1,1'-diiodoferrocenylene was in-situ prepared from reaction of CHI3 PPh3,t-BuOK and ferrocenecarboxaldehyde,further reaction with t-BuOK or n-BuLi gave the title compounds.

  17. One-Pot, Four-Step Organocatalytic Asymmetric Synthesis of Functionalized Nitrocyclopropanes.

    Science.gov (United States)

    Zaghi, Anna; Bernardi, Tatiana; Bertolasi, Valerio; Bortolini, Olga; Massi, Alessandro; De Risi, Carmela

    2015-09-18

    The asymmetric synthesis of functionalized nitrocyclopropanes has been achieved by a one-pot, four-step method catalyzed by (S)-diphenylprolinol TMS ether, which joins two sequential domino reactions, namely a domino sulfa-Michael/aldol condensation of α,β-unsaturated aldehydes with 1,4-dithiane-2,5-diol, and a domino Michael/α-alkylation reaction of the derived chiral dihydrothiophenes with bromonitromethane. The title compounds were obtained in 27-45% yields, with high levels of diastereoselectivity (93:7 to 100:0 dr) and generally good enantioselectivities (up to 95:5 er). PMID:26317611

  18. One-Pot Synthesis of Tetraphene and Construction of Expanded Conjugated Aromatics.

    Science.gov (United States)

    Wang, Jianbo; Yao, Jinzhong; Wang, Hailong; Chen, Hao; Dong, Jingcheng; Zhou, Hongwei

    2016-06-17

    Acene derivatives as a class of polycyclic aromatic hydrocarbons have attracted considerable interest because of their outstanding semiconductor properties. We developed a one-pot synthesis for fully conjugated tetraphene via a sequence of propargyl-allenyl isomerization, phosphine addition, intramolecular Wittig reactions, and Diels-Alder cyclization reactions. The derivative-conjugated aromatic compounds including carbazole or triphenylamine have been constructed via Pd-catalyzed coupling reaction with dibromotetraphene. These compounds show superior photophysical and electrochemical properties, which make them possible candidates for optoelectronic conjugated materials.

  19. ZSM-5催化一锅法合成3-(5’-取代-2’-苯并噁唑基)-7-二乙基氨基-2H-1-苯并吡喃-2-酮%One-Pot Synthesis of 3-(5'-Subsituted-benzoxazol-2'-yl)-7-diethyl-amino-chromen-2-one Catalyzed with ZSM-5

    Institute of Scientific and Technical Information of China (English)

    蒋绍亮; 韩亮

    2012-01-01

    3-(5'-Subsituted-benzooxazol-2'-yl)-7-diethylamino-chromen-2-ones were prepared by one-pot three-component reaction of 4-diethylaminosalicylaldehydes, ethyl cyanoacetate and o-aminophenols in refluxing rc-butanol catalyzed by ZSM-5. This method has advantages of better yields and more environment-friendly process compared with that catalyzed by liquid catalysts.%以绿色环保的固体酸ZSM-5分子筛为催化剂,正丁醇为溶剂,4-位取代邻氨基苯酚、4-二乙氨基水杨醛和氰乙酸乙酯三组分一锅法合成了香豆素类化合物3-(5’-取代-2’-苯并噁唑基)-7-二乙基氨基-2H-1-苯并吡喃-2-酮.与液体酸催化相比,该方法具有收率更高、环境友好等优点.

  20. An Efficient Method For The One-Pot, Four-Component Benzaldehyde Based Synthesis of 3-Methyl-1,4-Diphenyl-7,8-Dihydro-1H-Furo[3,4-E]Pyrazolo[3,4-B]Pyridin-5(4H-Ones Catalyzed by Alum in Environment-Friendly Media.

    Directory of Open Access Journals (Sweden)

    Sadif A. Shirvan

    2014-03-01

    Full Text Available A mild and efficient method for the synthesis of 3-methyl-1,4- diphenyl-7,8-dihydro-1H-furo[3,4-e]pyrazolo[3,4-b]pyridin-5(4H-one derivatives via one-pot, four-component reaction of aromatic aldehydes, tetronic acid, 3-aminobut-2-enenitrile, and phenylhydrazine is described using Alum as catalyst. The features of this procedure are mild reaction conditions, excellent yields, short reaction time, and operational simplicity.

  1. Recyclable Magnetite Nanoparticle Catalyst for One-Pot Conversion of Cellobiose to 5-Hydroxymethylfurfural in Water

    Directory of Open Access Journals (Sweden)

    Anuja Bhalkikar

    2015-01-01

    Full Text Available Environmentally benign and easily recoverable magnetite nanoparticles (Fe3O4 NPs were demonstrated to catalyze the one-pot conversion of cellobiose, a glucose disaccharide, to 5-hydroxymethylfurfural (5-HMF. The conversion was achieved in water under hydrothermal conditions. The catalytic activity of Fe3O4 NPs surpassed those of iron (II and iron (III chlorides in this reaction. Optimized cellobiose conversion reactions catalyzed with Fe3O4 NPs gave the highest 5-HMF yields of 23.4 ± 0.6% at 160°C for 24 hours. After three reuses, the Fe3O4 NP catalyst retained its catalytic activity with similar 5-HMF yields, demonstrating the recyclability of this eco-friendly catalyst in water.

  2. Formylation of Alcohol with Formic Acid under Solvent-Free and Neutral Conditions Catalyzed by Free I2 or I2 Generated in Situ from Fe(NO3)3·9H2O/NaI%无溶剂中性条件下分子I2或Fe(NO3)3·9H2O/NaI原位生成的I2催化醇与甲酸甲酰化反应

    Institute of Scientific and Technical Information of China (English)

    Rostami AMIN; Khazaei ARDESHIR; Alavi-Nik HEIDAR ALI; Toodeh-Roosta ZAHRA

    2011-01-01

    Different alcohols were formylated by formic acid under solvent-free conditions in the presence of iodine as the catalyst with good-to-high yields at room temperature.I2 generated in situ from Fe(NO3)3·9H2O/NaI also catalyzed the formylation of the alcohols under solvent-free conditions.This gives a green and efficient reaction at room temperature,in which the use of toxic and corrosive molecular I2 is avoided.

  3. 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.

  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. Four-component one-pot synthesis of unsymmetrical polyhydroquinoline derivatives using 3-methyl-1-sulfonic acid imidazolium hydrogen sulfate as a catalyst

    Institute of Scientific and Technical Information of China (English)

    Nader Ghaffari Khaligh

    2014-01-01

    3-Methyl-1-sulfonic acid imidazolium hydrogen sulfate has been used as an efficient, halogen-free, and reusable Brönsted acidic ionic liquid catalyst for the synthesis of ethyl-4-aryl/heteryl- hexahy-dro-trimehtyl-5-oxoquinoline-3-carboxylates via the one-pot condensation of dimedone with ar-yl/heteryl aldehydes, ethyl acetoacetate, and ammonium acetate under solvent-free conditions. This method has the advantage of being clean and simple, as well as providing the desired product in high yield over a short reaction time. Furthermore, the catalyst could be recycled and reused four times without any discernible reduction in activity.

  6. ZnO-Nanoparticles: Efficient and Reusable Heterogeneous Catalyst for One-Pot, Four-Component Synthesis of 2H-indazolo(2,1-b) phthalazine-triones

    International Nuclear Information System (INIS)

    ZnO nanoparticles as efficient and reusable catalyst for the synthesis of 2H indazolo(2,1-b)phthalazine-triones from the one-pot, four-component reaction of arylaldehydes, hydrazine monohydrate, phthalic anhydride, dime done under solvent-free conditions with short reaction times is described. The ZnO nanoparticles can be reused several times without significant loss of its catalytic activities. (author)

  7. Synthesis of benzo[g]indeno[2,1-b]quinoline derivatives via four-component and one-pot synthesis in presence of 3-methyl-1-sulfonic acid imidazolium hydrogen sulfate

    Institute of Scientific and Technical Information of China (English)

    Nader Ghaffari Khaligh

    2014-01-01

    A simple and facile synthesis of 12-arylbenzo[g]indeno[2,1-b]quinoline-6,11,13-trione deriv-atives was accomplished by the one-pot condensation of 2-hydroxynaphthalene-1,4-dione, aryl aldehydes, 2H-indene-1,3-dione, and ammonium acetate under solvent-free conditions in the presence of a Brönsted ionic liquid catalyst, namely 3-methyl-1-sulfonic acid imidazolium hydrogen sulfate.

  8. Enantioselective solvent-free Robinson annulation reactions

    Indian Academy of Sciences (India)

    D Rajagopal; R Narayanan; S Swaminathan

    2001-06-01

    The enantioselective cyclization of the prochiral cyclic substrates 1 to 7 and 26, can be carried out in the neat using -proline as catalyst. The substrates 18 to 22 and 27 could not be cyclized with S-proline but could be cyclized with a mixture of -phenylalanine and -camphorsulphonic acid. The enantioselective cyclization of prochiral acyclic triones 45 and 47 and also the racemic tricarbonyl compounds 54 to 57 could also be carried out in the \\text{neat} using -proline as catalyst. The optically active enediones obtained in the above cyclizations could also be obtained directly from 1,3-diones or 2-hydroxymethylene cycloalkanones in a one-pot reaction with methyl vinyl ketone (MVK) and S-proline in the absence of solvents. 13C NMR studies of the one-pot synthesis of S-11 and S-14 reveal that the annulations involve initial formation of an acid-base complex followed by a Michael reaction and then an enantioselective cyclization. Such enantioselective cyclizations probably occur on the surface of -proline crystals.

  9. Solvent-free ball-milling subcomponent synthesis of metallosupramolecular complexes.

    Science.gov (United States)

    Giri, Chandan; Sahoo, Prasit Kumar; Puttreddy, Rakesh; Rissanen, Kari; Mal, Prasenjit

    2015-04-20

    Subcomponent self-assembly from components A, B, C, D, and Fe(2+) under solvent-free conditions by self-sorting leads to the construction of three structurally different metallosupramolecular iron(II) complexes. Under carefully selected ball-milling conditions, tetranuclear [Fe4 (AD2 )6 ](4-) 22-component cage 1, dinuclear [Fe2 (BD2 )3 ](2-) 11-component helicate 2, and 5-component mononuclear [Fe(CD3 )](2+) complex 3 were prepared simultaneously in a one-pot reaction from 38 components. Through subcomponent substitution reaction by adding subcomponent B, the [Fe4 (AD2 )6 ](4-) cage converts quantitatively to the [Fe2 (BD2 )3 ](2-) helicate, which, in turn, upon addition of subcomponent C, transforms to [Fe(CD3 )](2+) , following the hierarchical preference based on the thermodynamic stability of the complexes.

  10. 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.

  11. Oligoquinolines under Solvent-free Microwave Irradiation

    International Nuclear Information System (INIS)

    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

  12. GREENER REACTIONS UNDER SOLVENT FREE CONDITIONS

    Directory of Open Access Journals (Sweden)

    Hiren M. Marvaniya

    2011-06-01

    Full Text Available The toxicity and volatile nature of many organic solvents, particularly chlorinated hydrocarbons that are widely used in huge amounts for organic reactions have posed a serious threat to the environment. Thus, design of solventless catalytic reaction has received tremendous attention in recent times in the area of green synthesis. A solvent-free or solid state reaction may be carried out using the reactants alone or incorporating them in clays, zeolites, silica, alumina or other matrices to achieve high degree of stereoselectivity in the products, to reduce byproducts, to maximize rate of reaction. We illustrate the environmentally benign approach to 1,2-Oxazine-2- oxides, Michael addition, Wohl–Ziegler reaction, Acylation, Heck reaction, Tishchenko reaction, Diels– Alder reaction, Reformatsky and Luche Reaction, Oxidative coupling Reaction, Synthesis of chalcones, Synthesis of Dihydropyrimidinones

  13. Boehmite nanoparticle catalyst for the one-pot multicomponent synthesis of 3,4-dihydropyrimidin-2-(1H)-ones and thiones under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Ali Keivanloo; Mahdi Mirzaee; Mohammad Bakherad; Atena Soozani

    2014-01-01

    A simple, green, and efficient synthesis protocol for the synthesis of 3,4-dihydropyrimidin-2-(1H)-ones using boehmite nanoparticles as catalyst was developed. It did not use any toxic metal cata-lysts or corrosive acidic reagents. The method gave good to excellent yields and has short reaction time, operational simplicity, and a recyclable catalyst.

  14. Cu-Pd/γ-Al2O3催化硝基苯和乙醇反应一锅法合成2-甲基喹啉%Cu-Pd/γ-Al2O3 catalyzed one-pot synthesis of 2-methylquinoline from nitrobenzene and ethanol

    Institute of Scientific and Technical Information of China (English)

    丰枫; 项益智; 汪小华; 马磊; 卢春山; 张群峰; 许孝良; 李小年

    2011-01-01

    在5%Cu-5%Pd/Y-A12O3催化剂作用下,由硝基苯和乙醇反应一锅法合成了2-甲基喹啉.实现了乙醇与硝基苯转移加氢、乙醛缩合、苯胺与不饱和醛加成、脱水环化、脱氢等多步反应的耦合.极大地简化了2-甲基喹啉的合成工艺.相比较传统的化学合成方法,由于避免了使用无机酸碱或均相金属络合物作为催化剂,该方法环境更加友好,解决了均相金属络合物催化剂分离、回收困难的问题.在优化的反应条件:使用1 g催化剂,硝基苯15mL,乙醇60mL,水30 mL,T=453 K,P=3.5 MPa,反应时间为12 h时,2-甲基喹啉的收率达66.4%.%One-pot synthesis of 2-methylquoinline from nitrobenzene and ethanol was realized over 5%Cu-5%Pd/y-A12O3 catalyst. The reactions of hydrogen transfer hydrogenation from ethanol to nitrobenzene, aldol-condensation of aldehyde, Michae-addition of aniline and unsaturated aldehydes, dehydration-cyclization, and dehydrogenation are combined successfully, which thus significantly simplified the production procedure of 2-methylquinoline. In comparison with the traditional chemical synthesis routes, the use of inorganic acid or homogeneous metal complex as the catalyst was eliminated. Therefore, this method is more environmentally friendly, or can solve the problems of separation and recovery of homogeneous metal complex catalyst. Under the optimal reaction conditions: 1 g 5%Cu-5%Pd/Y-Al2O3 catalyst, 15 mL nitrobenzene, 60 mL ethanol, 30 mL water, T= 453 K, P = 3.5 Mpa, and 12 h reaction time, the yield of 2-methylquinoline as high as 66.4% was obtained.

  15. 无溶剂体系中固定化脂肪酶Candida sp.99-125催化合成油酸低碳醇酯%Immobilized-Lipase (Candida sp.99-125)-Catalyzed Esterification of Alkyl Oleates in Solvent-free Systems

    Institute of Scientific and Technical Information of China (English)

    仲蕙; 方正; 邹宝华; 李昕; 郭凯

    2013-01-01

    采用固定化脂肪酶Candida sp.99-125在无溶剂体系中催化合成油酸低碳醇酯,考察了加酶量、温度、酸醇摩尔比和醇结构对油酸酯化率的影响.结果表明,加酶量为底物质量的3%,最适温度为20℃,酸与醇摩尔比为1∶1,甲醇对该酶有一定的毒性,由于空间位阻效应,该酶对伯醇具有高选择性,对仲醇、叔醇的选择性低,且对长链脂肪酸催化活性高,对带支链的多元酸、多元醇活性低.该酶重复使用5次,酶活性基本没有降低.与传统的化学法相比,用该酶催化合成酯类化合物的色泽更浅.%The esterification between oleic acid and alkyl alcohols in solvent-free systems were catalyzed by an immobilized lipase from Candida sp.99-125.The effects of several factors including enzyme concentration,temperature,molar ratio of oleic acid to alkyl alcohols,and structure of alcohols have been also investigated.The results indicated that the reactions catalyzed by lipase at 20 ℃ with the presence of 3 % (mass fraction)lipase,a 1 ∶ 1 molar ratio of oleic acid to alcohols,afforded products in high yields.Methanol has certain toxicity on the activity of the lipase.The enzyme showed high selectivity to primary alcohols and low selectivity to secondary and tertiary alcohols because of the sterical effect.It showed high activity to long chain fatty acids and low activity to polybasic acids and polyhydric alcohols with branched chain.The lipase showed no appreciable loss in activity after being continuously operated for 5 times.The enzymatic synthesis gave purer products,compared with the conventional chemical system.

  16. Synthesis of 14-Fluorophenyl-14H-Dibenzo[a,j]xanthenes and Their Derivatives under Microwave Irradiation and Solvent-free Conditions%Synthesis of 14-Fluorophenyl-14H-Dibenzo[a,j]xanthenes and Their Derivatives under Microwave Irradiation and Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    金见安; 章健民; 商文丽; 朱仕正

    2011-01-01

    A facile and efficient synthesis of 14-fluorophenyl-14H-dibenzo[a,j]xanthenes has been developed by one-pot condensation of fluorinated benzaldehydes with β-naphthol in the presence of p-TSA·H2O under microwave irradiation and solvent-free conditions. These products are conveniently oxidized to 14-fluorophenyl-14-hydroxydibenzo[a,j]xanthenes by PbO2 in acetic acid in good yields.

  17. Direct application of gold nanoparticles to one-pot electrochemical biosensors.

    Science.gov (United States)

    Chen, Guifang; Tong, Hui; Gao, Tao; Chen, Yangyang; Li, Genxi

    2014-11-01

    Gold nanoparticles (AuNPs) have been widely employed for the fabrication of electrochemical biosensors. In most cases, AuNPs are immobilized on the surface of an electrode, so they are difficult to be regenerated, making the use of the biosensor unfriendly. In this work, by adopting AuNPs directly as the electrolytes, we have developed a novel AuNPs-based electrochemical detection system. In brief, AuNPs-catalyzed oxidation of glucose is combined with a HRP-catalyzed reaction as well as an electrocatalytic reaction to compose cascade reactions in the electrolyte. Thus, the intensity of the electrocatalytic signals has quantitative relation with the concentration of glucose, and favors the sensitive detection of glucose. Furthermore, because the catalysis of AuNPs may be blocked under the interaction with single-stranded DNA and unblocked in the presence of a complementary sequence, detection of DNA and even single-nucleotide polymorphism can thereby been achieved. This one-pot detection system can be operated and regenerated very easily, since all the components are integrated in the electrolytes of AuNPs, and the unmodified electrode can be reused after being rinsed. This concept by integrating the advantages of sensitive electrochemical detection with the easy-to-operate nanocolloidal system may also promote the development of other kinds of electrochemical biosensors. PMID:25300210

  18. One-Pot Synthesis of Dimethyl Carbonate from Supercritical CO2 Catalyzed by Using Metal Acetates Formulation Catalyst%金属醋酸盐复配催化剂催化超临界CO2一步法合成碳酸二甲酯

    Institute of Scientific and Technical Information of China (English)

    林春绵; 丁春晓; 张平; 徐明仙

    2012-01-01

    The synthesis of dimethyl carbonate (DMC) from carbon dioxide is one of the important routes of the resourcization of carbon dioxide. Because of its particular solubility and transitivity, the supercritical carbon dioxide(SC-CO2) can be used as both reagent and solvent in the reaction. In this experiment, metal acetates K2CO3 and KI were used as catalysts for the one-pot synthesis of DMC with SC-CO2, propylene oxide (PO) and methanol(CH3OH) as raw materials. The influences of catalyst dosage, FCH3OH:VPO, temperature (from 130℃ to 170℃), pressure(from 2 to 14 MPa) and reaction time were investigated. Products were analyzed by gas chromatography with the use of internal standard method. When the multiplex catalyst with the mass ratio of K2CO3:KI:Zn(CH3COO)2=l:l:2 was used, under the suitable reaction conditions (catalyst dosage 4%, PCH3OH:VPO=8:1, 160℃, 7.4 MPa, reaction time 4 hours), the conversion of propylene oxide could reach 95% and the yield of DMC could reach 54.3%.%由CO2合成碳酸二甲酯(DMC)是CO2资源化的重要途径之一,超临界CO2因具有独特的溶解和传递性能,在合成反应中可既作反应物,又作反应溶剂.本实验以超临界CO2、环氧丙烷和甲醇作为反应物,选用金属醋酸盐与K2CO3、KI复合催化一步合成DMC.在温度130-170℃、CO2压力2~14 MPa条件下,考察了催化剂用量、物料配比、温度、压力、反应时间等条件对DMC产率的影响,产物采用气相色谱以内标法进行定量分析.结果表明,当醋酸锌复合催化剂配比为K2CO3∶KI∶Zn(CH3COO)2=1∶1∶2时,在合适的反应条件下(催化剂用量4%,物料配比8∶1,160℃、7.4MPa,反应4 h),环氧丙烷转化率可达95%,DMC产率可达54.3%.

  19. Iodine Supported on 3-Aminopropyl Silica Gel as Efficient Catalyst for Acetylation of Alcohols under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    MAHDAVI Hossein; GHAEMY Mosa; ZERAATPISHEH Fatemeh

    2009-01-01

    3-Aminopropyl silica gel (I2/APSG) was found to catalyze the acetylation of alcohols and phenols efficiently with acetic anhydride. The reaction is mild and selective with high yields. A wide variety of alcohols and phenols are selectively converted into the corresponding acetates using I2/APSG under solvent-free conditions at room tem-perature.

  20. 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.

  1. Solvent Free Synthesis of Chalcones and their Antibacterial Activities

    OpenAIRE

    K. Rajendra K. Saini; S. Amit Choudhary; Joshi, Yogesh C.; Joshi, P.

    2005-01-01

    The solvent free synthesis of six chalcones was carried out by grinding the piperanal and the acetophenone (unsubstituted, 4-methyl, 4-methoxy, 4-bromo, 4-nitro, 3-chloro) in the presence of solid sodium hydroxide with a mortar and pestle. In general, the chalcones were obtained in high yield and high purity. Minor quantities of Ketol and Michael addition product were easily removed by recrystallization. The result indicates a correlation between the success of the solvent-free synthesis and ...

  2. A Facile Three-Component One-Pot Synthesis of Structurally Constrained Tetrahydrofurans, Which Are t-RNA Synthetase Inhibitor Analogues

    Institute of Scientific and Technical Information of China (English)

    LU,Chong-Dao; CHEN,Zhi-Yong; HU,Wen-Hao; MI,Ai-Qiao

    2004-01-01

    @@ A one-pot procedure for the efficient synthesis of a small library of t-RNA inhibitor analogues was developed. Thus,Rh2(OAc)4 catalyzed three-component 1,3-dipolar cycloaddition reactions of carbonyl ylides derived from diazoindan-1,3-dione and aldehydes with other dipolarophiles in 1,1,2,2-tetrachloroethane at 80 ℃ gave ring fused tetrahydrofurans having three stereocenters in good yield.

  3. 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.

  4. Efficient One-pot Synthesis of Pyrrolo[2,1-a]isoquinoline and Pyrrolo[1,2-a]quinoline Derivatives

    Institute of Scientific and Technical Information of China (English)

    LIU Zhen-ming; WU Lei; SUN Jing; YAN Chao-guo

    2012-01-01

    A one-pot sequential reaction for efficient synthesis of pyrrolo[2,1-a]isoquinoline and pyrrolo[1,2-a]-quinoline derivatives has been developed.The reaction included firstly the Cu-catalyzed three-component reaction of isoquinoline(quinoline),acetylenedicarboxylate and alkynylbenzene and then Cs2CO3-promoted intramolecular cyclization reaction of initially formed 1-alkeny1-2-alkynyl-1,2-dihydroisoquinoline(1,2-dihydroquinoline).

  5. Synthesis of spiro[pyrazolo[3,4-] pyridine-4,3'-indoline] and spiro [benzo[ℎ]pyrazolo[3,4-]quinoline-4,3'-indoline] derivatives using wet cyanuric chloride under solvent-free conditions

    Indian Academy of Sciences (India)

    Zhikui Yin; Limin Yang; Liqiang Wu

    2013-05-01

    A simple and efficient synthesis of spiro[pyrazolo[3,4-]pyridine-4,3'-indoline] and spiro[benzo[ℎ] pyrazolo[3,4-]quinoline-4,3'-indoline] derivatives has been accomplished by the one-pot condensation of isatins, 3-methyl-1-phenyl-1-pyrazol-5- amine and Meldrum’s acid or 2-hydroxy-1,4-naphthoquinone in the presence of wet cyanuric chloride as a catalyst under solvent-free conditions.

  6. Multicomponent, solvent-free synthesis of 12-aryl-8,9,10,12-tetrahydrobenzo[]-xanthen-11-one derivatives catalysed by cyanuric chloride

    Indian Academy of Sciences (India)

    Zhan-Hui Zhang; Peng Zhang; Shu-Hong Yang; Hong-Juan Wang; Jia Deng

    2010-05-01

    An efficient and direct protocol for the preparation of 12-aryl-8,9,10,12-tetrahydro-benzo[] xanthen-11-one derivatives employing a three-component one-pot reaction of aryl aldehydes, 2-naphthol and cyclic 1,3-dicarbonyl compounds in the presence of a catalytic amount of cyanuric chloride (2,4,6-trichloro-1,3,5-triazine, TCT) under solvent-free conditions is described. The desired products are obtained in high yields with short reaction times.

  7. An eco-sustainable green approach for the synthesis of propargylamines using LiOTf as a reusable catalyst under solvent-free condition

    Indian Academy of Sciences (India)

    Someshwar D Dindulkar; Baek Kwan; Kwon Taek Lim; Yeon Tae Jeong

    2013-01-01

    An efficient process has been developed for the synthesis of propargylamines via a threecomponent coupling reaction of aldehyde, secondary alicyclic amine and alkyne (A3) under solvent-free condition using lithium triflate (LiOTf) as expeditious reusable catalyst. This one-pot transformation generates one C-C and one C-N bond, which presumably proceeds by lithium acetylide as well as formation of iminium ion in situ and then undergoes nucleophilic addition to the iminium ion to give the propargyl amine. The solventfree condition, easy recovery of the catalyst, simple, user-friendly and quantitative yield in short time renders the protocol economic and reasonable.

  8. Synthesis of TP3 Fragment via One Pot Strategy and Its Immune Regulatory Activity

    Institute of Scientific and Technical Information of China (English)

    WANG Li-feng; CHEN Jie; SHAN Hui-jie; LI Wei

    2005-01-01

    We have modified the previously described one-pot peptide synthesis method. The modified method has been successfully applied to the synthesis of TP3. Furthermore, the immune regulatory activity of TP3 has been characterized. The results show that the modified one-pot method can be used to synthesize the biological active peptide with the advantages of low cost and high productivity. Moreover, TP3 has a higher immune regulatory activity than TP5.

  9. One pot preparation of silver nanoparticles decorated TiO2 mesoporous microspheres with enhanced antibacterial activity.

    Science.gov (United States)

    Chen, Yuemei; Deng, Yuanming; Pu, Yitao; Tang, Bijun; Su, Yikun; Tang, Jiaoning

    2016-08-01

    We report a simple "one-pot" solvothermal preparation of silver nanoparticles (Ag NPs) decorated mesoporous titania (TiO2) microspheres as an effective antibacterial agent. TBOT as Ti source was hydrolyzed and crystallized in media composed of acetic acid and ethanol, in which esterification catalyzed by TBOT occurred for in-situ "controlled water release". AgNO3 as Ag source was reduced by ethanol to form Ag NPs embedded in the TiO2 microspheres. The effect of AgNO3 and HAc on the morphology of Ag/TiO2 was investigated. The Ag/TiO2 with various Ag content showed excellent antibacterial activities with extremely low minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against Escherichia coli and Staphylococcus aureus when compared with colloidal Ag NPs. PMID:27157724

  10. 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.

  11. 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)

  12. Solvent-free extraction of food and natural products

    OpenAIRE

    Fabiano-Tixier, Anne-Sylvie; Vian, Maryline; Allaf, Tamara; Vorobiev, Eugene

    2015-01-01

    This review presents useful and green techniques of solvent-free extraction used in ancient times, such as extraction of olive oil and citrus essential oil, and innovative techniques, such as pulsed electric field, microwave, instantaneous controlled pressure drop, and extrusion. We discuss the devices, their applications, mechanisms, and parameters influencing sample preparation prior to analysis of natural products.

  13. Solvent-free synthesis of some ethyl arylglyoxylates

    Institute of Scientific and Technical Information of China (English)

    Ji Ming Xiang; Bao Lin Li

    2009-01-01

    An efficient and convenient approach to synthesize of ethyl arylglyoxylates by solvent-free grinding was described. Eight ethyl arylglyoxylates had been synthesized by this method, this method provided several advantages such as little pollution, high yield, good selectivity, and simple workup procedure, their structures were confirmed by IR, 1HNMR.

  14. An efficient synthesis of quinolines under solvent-free conditions

    Indian Academy of Sciences (India)

    Mihir K Chaudhuri; Sahid Hussain

    2006-03-01

    An efficient synthesis of substituted quinolines has been achieved in a one-pot reaction from -nitrobenzaldehyde and enolizable ketones using SnCl2.2H2O as the reductant under microwave irradiation without any solvent or catalyst.

  15. Highly efficient synthesis of β-amino esters via Mannich-type reaction under solvent-free conditions using ZnCl2 catalyst

    Institute of Scientific and Technical Information of China (English)

    Xue Ming Chen; Xing Shu Li; Albert S.C. Chan

    2009-01-01

    β-Amino esters were synthesized via ZnCl2-catalyzed Mannich-type reaction of imines and malonate esters under solvent-free conditions in 6 min.The β-amino ester was converted into the corresponding aspartic acid derivatives.

  16. Green chemistry approaches to the regioselective synthesis of spiro heterobicyclic rings using iodine as a new and efficient catalyst under solvent-free conditions.

    Science.gov (United States)

    Prajapati, Dipak; Bhuyan, Debajyoti; Gohain, Mukut; Hu, Wenhao

    2011-02-01

    Iodine catalyzes the pseudo four-component reaction of an aldehyde, a urea or thiourea, and cyclic 1,3-dicarbonyl compounds under microwave irradiation in a solvent-free condition to yield various σ symmetric spiro heterobicyclic rings in excellent yields. PMID:20364370

  17. Green chemistry approaches to the regioselective synthesis of spiro heterobicyclic rings using iodine as a new and efficient catalyst under solvent-free conditions.

    Science.gov (United States)

    Prajapati, Dipak; Bhuyan, Debajyoti; Gohain, Mukut; Hu, Wenhao

    2011-02-01

    Iodine catalyzes the pseudo four-component reaction of an aldehyde, a urea or thiourea, and cyclic 1,3-dicarbonyl compounds under microwave irradiation in a solvent-free condition to yield various σ symmetric spiro heterobicyclic rings in excellent yields.

  18. Magnesium bistrifluoromethanesulfonimide as an efficient catalyst for the hydroalkylation of aromatic olefins with 1,3-diketones under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Hong She Wang; Wei Xing Zhao

    2011-01-01

    An efficient magnesium bistrifluoromethanesulfonimide [Mg(NTf2)2] catalyzed hydroalkylation of aromatic olefins with 1,3-diketones under solvent-free conditions has been developed. The reactions proceed smoothly to give the desired products in good yields in short reaction times.

  19. Application of an ortho-Formylation Reaction in One-pot Procedures and Natural Product Syntheses

    OpenAIRE

    2009-01-01

    This thesis describes the transformation of phenols into ortho-hydroxycinnamates, salicylamines, benzoxazines, and salicylnitriles in good overall yields by simple, regioselective, and one-pot procedures using a combination of MgCl2-Et3N as a base system. These one-pot processes are more economically and environmentally benign than those methods previously reported. The MgCl2-Et3N base system was also used in a regioselective Mannich reaction. Moreover, the first total synthesis of (±)-pow...

  20. Amberlyst-15 catalyzed synthesis of alkyl/aryl/heterocyclic phosphonates

    Institute of Scientific and Technical Information of China (English)

    U.M. Rao Kunda; V.N. Reddy Mudumala; C.S. Reddy Gangireddy; B.R. Nemallapudi; K.N. Sandip; S.R. Cirandur

    2011-01-01

    A novel and efficient procedure for the synthesis of alkyl phosphonates through one pot condensation of alkyl halide and tri-alkyl/aryl phosphite in the presence of Amberlyst-15 as catalyst under solvent free conditions was applied. It demonstrated several advantages such as good yields of products, simple operation, convenient separation and inexpensive catalyst.

  1. Cyclotrimerization of nitriles catalyzed by Li3N

    Institute of Scientific and Technical Information of China (English)

    DENG Zhaoxiang; QIU Wenfeng; LI Weijia; LI Yadong

    2004-01-01

    Nitriles were unexpectedly trimerized into s-triazines or amino-pyrimidines in high yields in the presence of catalytic amount of Li3N, resulting in a simple, solvent-free and easy-to-scale-up one-pot way to synthesize s-triazines and 4-amino-pyrimidines with high yield.

  2. One-pot multi-reaction processes: synthesis of natural products and drug-like scaffolds

    OpenAIRE

    Calder, Ewen D D; Grafton, Mark W.; Sutherland, Andrew

    2014-01-01

    One-pot multi-reaction processes involving Overman rearrangements, metathesis cyclizations, and Diels–Alder reactions have been developed for the rapid and efficient synthesis of amino-substituted carbocyclic and heterocyclic compounds. This account describes the development and optimization of these processes, as well as their applications in the synthesis of natural products and drug-like scaffolds.

  3. One-pot four component synthesis of novel 3-furyl coumarin derivatives

    Indian Academy of Sciences (India)

    Venkata Prasad Jalli; Suvratha Krishnamurthy; Tetsuji Moriguchi; Akihiko Tsuge

    2016-02-01

    Efficient and facile synthesis of 3-furyl coumarin derivatives have been achieved by reaction of 4-chloro-3-formylcoumarin, secondary amines, dialkyl acetylenedicarboxylates and diversely substituted isocyanides using four component, one-pot reaction. All the products were isolated as yellow color fluorescent solids by column chromatography in quantitative yield and characterized with 1H NMR, 13C NMR, IR and FAB mass.

  4. An efficient green synthesis of dispirohydroquinolines via a diastereoselective one-pot eight-component reaction

    Institute of Scientific and Technical Information of China (English)

    Sajjad Salahia; Malek Taher Maghsoodloua; Nourallah Hazeria; Mojtaba Lashkaria; Santiago Garcia-Granda; Laura Torre-Fernandez

    2015-01-01

    The one-pot eight-component reaction between Meldrum's acid, an aromatic aldehyde, and an aryl amine was achieved in the presence of citric acid catalyst. The corresponding dispirohydroquino-lines were obtained in good yields with excellent diastereoselectivity. This method is a combination of the Knoevenagel and Michael reactions.

  5. Reactivity-based One-pot Synthesis of Immunosuppressive Glycolipids from the Caribbean Sponge Plakortis simplex

    Institute of Scientific and Technical Information of China (English)

    L(U), Guokai; WANG, Peng; LIU, Qingchao; ZHANG, Zaihong; ZHANG, Wei; LI, Yingxia

    2009-01-01

    The first synthesis of three natural glycolipid simplexides 1a-1c, which were isolated from the marine sponge Plakortis simplex and claimed to inhibit T cell proliferation, has been concisely accomplished by a reactivity-based one-pot synthetic strategy under the use of p-toluenethioglycoside (STol) donors.

  6. Facile one-pot synthesis of unsymmetrical ureas, carbamates, and thiocarbamates from Cbz-protected amines.

    Science.gov (United States)

    Kim, Hee-Kwon; Lee, Anna

    2016-07-26

    A novel one-pot synthesis of unsymmetrical ureas, carbamates and thiocarbamates from Cbz-protected amines has been developed. In the presence of 2-chloropyridine and trifluoromethanesulfonyl anhydride, isocyanates are generated in situ, which facilitate rapid reaction with amines, alcohols, and thiols to afford the corresponding ureas, carbamates and thiocarbamates in high yields. PMID:27406041

  7. A Facile Synthesis of Polysubstituted Pyrroles by One-Pot Three-Component Reaction

    OpenAIRE

    Anaraki-Ardakani, Hossein; Noei, Maziar; Karbalaei-Harofteh, Mina; Zomorodbakhsh, Shahab

    2012-01-01

    A new and efficient one-pot synthesis of polysubstituted pyrrole derivatives by three-component reaction between dialkyl acetylenedicarboxylates, triphenylphosphine, 2-aminopyridin derivatives in the presence of arylglyoxals is described. The reactions were performed in dichloromethane at room temperature and neutral conditions and afforded high yields of products.

  8. Organocatalytic One-Pot Asymmetric Synthesis of Thiolated Spiro-γ-lactam Oxindoles Bearing Three Stereocenters.

    Science.gov (United States)

    Huang, Xin; Liu, Miao; Pham, Kenny; Zhang, Xiaofeng; Yi, Wen-Bin; Jasinski, Jerry P; Zhang, Wei

    2016-07-01

    The first asymmetric synthesis of spiro-γ-lactam oxindoles bearing three stereocenters is reported. One-pot thiol-Michael/Mannich/lactamization reactions promoted by a recyclable fluorous bifunctional cinchona alkaloid/thiourea organocatalyst afford products in moderate to good yields with up to 95% ee and 6:1 dr. PMID:27258150

  9. Platinum-Copper Nanoframes: One-Pot Synthesis and Enhanced Electrocatalytic Activity.

    Science.gov (United States)

    Yu, Xiaofei; Li, Lanlan; Su, Yanqiu; Jia, Wei; Dong, Lili; Wang, Dingsheng; Zhao, Jianling; Li, Yadong

    2016-03-24

    Platinum-copper nanoframes were produced from copper nanoparticles by a one-pot synthesis method. The growth mechanism was thoroughly studied by experiment and theoretical calculations. Owing to the unique structure, Pt-Cu nanoframes exhibited significantly enhanced catalytic activity toward the electro-oxidation of methanol compared to commercial Pt black. PMID:26880582

  10. Effect on nerve structures of functionalized gold-chitosan nanoparticles obtained by one pot synthesis

    Directory of Open Access Journals (Sweden)

    Marius Dobromir

    2011-02-01

    Full Text Available Gold nanoparticles have potential applications in drug delivery, cancer diagnosis and therapy, food industry and environment remediation. However, little is known about their potential toxicity or fate in the environment. In this study we observed significant effects of functionalized gold-chitosan nanoparticles obtained by one pot synthesis on nerve structures of Wistar rats.

  11. One pot synthesis of cyclohexanone oxime from nitrobenzene using a bifunctional catalyst.

    Science.gov (United States)

    Rubio-Marqués, Paula; Hernández-Garrido, Juan Carlos; Leyva-Pérez, Antonio; Corma, Avelino

    2014-02-18

    Cyclohexanone oxime is formed from nitrobenzene with 97% yield in a one-pot reaction catalysed by palladium and gold nanoparticles on carbon. The reaction is carried out under hydrogen at 60 °C and the overall transformation involves a multi-step catalysed mechanism from which intermediates and catalytically active species have been identified.

  12. Microwave-assisted one-pot synthesis of benzothiazole and benzoxazole libraries as analgesic agents

    Indian Academy of Sciences (India)

    C Praveen; A Nandakumar; P Dheenkumar; D Muralidharan; P T Perumal

    2012-05-01

    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 moderate to good activity.

  13. 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.

  14. 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.

    2011-01-01

    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 analysi

  15. 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.

  16. 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.

  17. Cross-aldol condensation between cyclohexanone and aromatic aldehydes catalyzed by silicon dioxide supported phosphoric acid under solvent-free conditions%无溶剂条件下硅胶固载磷酸催化环己酮与芳香醛的缩合反应

    Institute of Scientific and Technical Information of China (English)

    裴强; 金春雪; 薛灵芬; 张小宁; 宋文姬

    2011-01-01

    Seven α,β-unsaturated ketones were synthesized from cross-aldol condensation between aromatic aldehydes and cyclohex-anone in the presence of silicon dioxide supported phosphoric acid under solvent-free conditions. It showed advantages of short reaction time (60 - ISO rain) and good yields (73.4%~92.7% ). This method was simple,fast,environmental friendly,and the catalyst could be reused.%以硅胶(mSiO2·nH2O)固载磷酸为催化剂,在无溶剂条件下催化环已酮与芳香醛的Cross-Aldol缩合反应,得到7个相应的α,β不饱和羰基化合物,反应时间短(60~150 min),产率高(73.4% ~ 92.7%).该方法操作简单,催化剂可重复使用,且对环境友好.

  18. Aldol Condensation of Tetrahydro-4H-pyran-4-one and Aromatic Aldehydes Catalyzed by NH2SO3 H Under Solvent-Free Conditions and Microwave Irradiation%无溶剂NH2SO3H催化下微波促进四氢吡喃-4-酮与芳香醛的Aldol缩合反应

    Institute of Scientific and Technical Information of China (English)

    薛蒙伟; 张敦林; 刘光祥; 李健

    2013-01-01

    以四氢吡喃-4-酮与芳香醛(1)为原料,NH2SO3H为催化剂,在无溶剂条件下,微波促进Aldol缩合反应合成了一系列3,5-二亚苄基四氢吡喃4-酮衍生物(收率72%~92%),其结构经1H NMR,IR,MS和元素分析确证.最佳反应条件为:1 12 mmol,NH2SO3H用量40 mol%,于300 W微波辐射2 min~3 min.%A series of 3,5-dibenzylidene-tetrahydropyran-4-one derivatives with yield of 72% ~ 92% were synthesized by Aldol condensation of tetrahydro-4H-pyran-4-one with aromatic aldehydes(1) using NH2SO3H as the catalyst under solvent-free condition and microwave irradiation.The structures were confirmed by 1H NMR,IR,MS and elemental analysis.The optimum reaction conditions were as follows:1 was 12 mmol,NH2SO3H amount was 40 mol%,microwave irradiation at 300 W for 2 min ~ 3 min.

  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. Zirconia-based catalyst for the one-pot synthesis of coumarin through Pechmann reaction.

    Science.gov (United States)

    Khan, Shahid Ali; Khan, Sher Bahadar; Asiri, Abdullah M; Ahmad, Ikram

    2016-12-01

    Coumarins play an important role in drug development with diverse biological applications. Herein, we present the synthesis of coumarin through Pechmann reaction by using zirconia-based heterogeneous catalysts (ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose) in a solvent-free condition at room temperature. ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose were identified through spectroscopic techniques such as FESEM, X-ray, EDS, XPS, and FT-IR. ZrO2-TiO2 showed the best catalytic performance while ZrO2/cellulose was inactive. The kinetic parameters were observed in a solvent-free condition as well as in toluene and ethanol. The temperature effect was extensively studied which revealed that increasing the temperature will increase the rate of reaction. The rate of reaction in a solvent-free condition, ethanol, and toluene were 1.7 × 10(-3), 1.7 × 10(-2), and 5.6 × 10(-3) g mol(-1) min(-1), respectively. PMID:27460593

  1. Zirconia-based catalyst for the one-pot synthesis of coumarin through Pechmann reaction

    Science.gov (United States)

    Khan, Shahid Ali; Khan, Sher Bahadar; Asiri, Abdullah M.; Ahmad, Ikram

    2016-07-01

    Coumarins play an important role in drug development with diverse biological applications. Herein, we present the synthesis of coumarin through Pechmann reaction by using zirconia-based heterogeneous catalysts (ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose) in a solvent-free condition at room temperature. ZrO2-TiO2, ZrO2-ZnO, and ZrO2/cellulose were identified through spectroscopic techniques such as FESEM, X-ray, EDS, XPS, and FT-IR. ZrO2-TiO2 showed the best catalytic performance while ZrO2/cellulose was inactive. The kinetic parameters were observed in a solvent-free condition as well as in toluene and ethanol. The temperature effect was extensively studied which revealed that increasing the temperature will increase the rate of reaction. The rate of reaction in a solvent-free condition, ethanol, and toluene were 1.7 × 10-3, 1.7 × 10-2, and 5.6 × 10-3 g mol-1 min-1, respectively.

  2. One-pot Synthesis of Lewis Acidic Ionic Liquids for Friedel-Crafts Alkylation

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Novel Lewis acidic ionic liquids containing thionyl cations and chloroaluminate anions were obtained by one-pot synthesis for the first time. Their acidities were determined by acetonitrile probe on IR spectrography. The ionic liquids were used as catalyst for Friedel-Crafts alkylation of benzene and 1-dodecene. The turnovers of 1-dodecene were higher than 99%. Monoalkylbenzene selectivity was 98%, while the 2-substituent product selectivity was 45%.

  3. A general and facile one-pot process of isothiocyanates from amines under aqueous conditions

    OpenAIRE

    Nan Sun; Bin Li,; Jianping Shao; Weimin Mo; Baoxiang Hu; Zhenlu Shen; Xinquan Hu

    2012-01-01

    A general and facile one-pot protocol for the preparation of a broad range of alkyl and aryl isothiocyanates has been developed from their corresponding primary amines under aqueous conditions. This synthetic process involves an in situ generation of a dithiocarbamate salt from the amine substrate by reacting with CS2 followed by elimination to form the isothiocyanate product with cyanuric acid as the desulfurylation reagent. The choice of solvent is of decisive importance for the successful ...

  4. One-Pot Synthesis of 1,8-Dioxo-octahydroxanthene Derivatives

    OpenAIRE

    Seyyedeh Naghmeh Sadat; Farhad Hatamjafari

    2015-01-01

    An efficient, simple and one-pot protocol for synthesis of 1,8-Dioxo-octahydroxanthene derivatives via multi-component reactions between dimedone and various aromatic aldehydes employing barium perchlorate as catalyst is described. The structural features of the synthesized compounds were characterized by IR and 1H NMR. The presented method is available, environmentally friendly, cheap and highly effective to give the products in good to excellent yields.

  5. An Efficient Four-Component,One-Pot Synthesis of Poly-Substituted Pyrimidines in Water

    Institute of Scientific and Technical Information of China (English)

    WANG,Zhongqing; GE,Zemei; CHENG,Tieming; LI,Runtao

    2009-01-01

    An efficient environmentally friendly synthesis of poly-substituted pyrimidines has been developed via a four-component,one-pot reaction of malononitrile,carbon disulfide,alkyl halide and S-alkylisothiouronium salt in water at room temperature.Water as solvent,mild reaction conditions,short reaction time,simple experimental procedures,broad scope of substrates and good yields are the main advantages of this method.

  6. Efficient one-pot four-component synthesis of fused thiazolopyridin-2-ones in ionic liquid

    Indian Academy of Sciences (India)

    Prashant Singh; Kamlesh Kumari; Gaurav Kaithwas; Gaurav Kaithwas

    2013-11-01

    An efficient one-pot synthesis of fused thiazolopyridinone derivatives (5-amino-6,7-diphenyl-4,7-dihydro-3H-thiazolo[4,5-b]pyridin-2-ones) by four-component reaction of aldehyde, benzylcyanide, ammonium acetate and thiazolidine-2,4-dione in ionic liquid is reported. This protocol has the advantages of environmental friendliness, higher yields, less reaction time, and convenient operation. Also, optimization of the synthesized compounds has been done using Hyperchem 8.0.

  7. Ir-Cu nanoframes: one-pot synthesis and efficient electrocatalysts for oxygen evolution reaction.

    Science.gov (United States)

    Pei, Jiajing; Mao, Junjie; Liang, Xin; Chen, Chen; Peng, Qing; Wang, Dingsheng; Li, Yadong

    2016-03-01

    Herein, we achieved successful synthesis of uniform Ir-Cu nanoframes with highly open structures by a facile one-pot strategy. The key to obtain alloy nanoframes was the careful control over the reduction and galvanic replacement reactions between different metals. The as-prepared Ir-Cu was proved to be an effective template for constructing trimetallic nanoframes. Furthermore, these highly open nanostructures exhibited excellent electrocatalytic performance toward oxygen evolution reaction in alkaline media. PMID:26864283

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

    International Nuclear Information System (INIS)

    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) 124I labelled iodaryl azides while minimising manipulation of radioactive materials. Purification of the [125I]iodoazido photoaffinity labels is achieved by high performance liquid chromatography. (author)

  9. One pot synthesis of 1-substituted tetrahydro--carbolines by Bischler–Napieralski cyclization

    Indian Academy of Sciences (India)

    Thokchom Prasanta Singh; Okram Mukherjee Singh

    2016-04-01

    A novel and facile one-pot synthesis of 1-substituted tetrahydro--carbolines by cyclocondensation of ketene ,–acetals with tryptamine in presence of InCl3 and TFA as co-catalysts by Bischler-Napieralski cyclization is described. The reaction involves formation of one C-N bond, one C-C bond and a new ring annulation over an indole moiety.

  10. 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.

  11. One-pot sequential alkynylation and cycloaddition: regioselective construction and biological evaluation of novel benzoxazole-triazole derivatives.

    Science.gov (United States)

    Srivastava, Ananya; Aggarwal, Leena; Jain, Nidhi

    2015-01-12

    Individually, benzoxazole and triazole moieties are of significant biological interest owing to their importance in drugs and pharmaceuticals. To assess their combined biological impact when woven into one molecule, we designed a novel, regioselective, multicomponent, one-pot (MCOP) approach for the construction of benzoxazole-linked triazoles. The synthesis has been achieved in two sequential steps involving copper-catalyzed alkynylation of benzoxazole followed by a 1,3-dipolar cycloaddition reaction. By combination of these two bioactive units into one core, a series of new benzoxazole-triazole scaffolds has been synthesized and subjected to in vitro antibacterial and anticancer evaluation. Tests against clinical isolates of Staphylococcus aureus and Escherichia coli showed potent Gram-negative activity for compounds 4{1,1,1}, 4{1,1,4}, and 4{1,2,1}. The cytotoxicity of the synthesized library was determined against three cancer cell lines: HeLa, SKBr3, and Hep G2. Compound 4{2,2,2} showed significant cytotoxicity against all the cell lines. These preliminary bioassay evaluations strongly suggest the promise and scope of these novel molecules as therapeutic agents in medical science.

  12. Solvent-free Synthesis of 5-Azacytosine with Microwave Activation

    Institute of Scientific and Technical Information of China (English)

    LIU Qi-bin; QU Gui-rong

    2004-01-01

    5-Azacytosine (4-amino-1,2-dihydro-1,3,5-triazin-2-one) is a very important intermediate in the synthesis of 5-azacytidine which showed remarkable bacteriostatic and cytostatic activity as well as against T-4 lymphoma and L-1210 leukemia in mice. Starting with N-cyanoguanidine (dicyandiamide) and formic acid, under the solvent-free microwave activation,we synthesized 5-azacytosine in short time (4min) with good yield (60.4%). The structure of the product was confirmed by 1HNMR and Elemental analysis.In this paper, a new and rapid synthesis of 5-azacytosine has been reported for the first time in microwave oven. N-cyanoguanidine (0.05tmol) and anhydride formic acid (0.18mol) were stirred well. Then irradiate the reaction mixture in microwave oven for the specified time (4min) under solvent-free condition. After the reaction was complete, the resulting solid was disperated in warm absolute ethanol (10ml), cooled to 0℃, filtered and dried in vacuum to yield the crude product. The pure product was obtained by recrystallization.

  13. Synthesis and Evaluation of Cu/SAPO-34 Catalysts for NH3-SCR 2: Solid-state Ion Exchange and One-pot Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Feng; Walter, Eric D.; Washton, Nancy M.; Szanyi, Janos; Peden, Charles HF

    2015-01-01

    Cu-SAPO-34 catalysts are synthesized using two methods: solid-state ion exchange (SSIE) and one-pot synthesis. SSIE is conducted by calcining SAPO-34/CuO mixtures at elevated temperatures. For the one-pot synthesis method, Cu-containing chemicals (CuO and CuSO4) are added during gel preparation. A high-temperature calcination step is also needed for this method. Catalysts are characterized with surface area/pore volume measurements, temperature programmed reduction (TPR), electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) spectroscopies, and scanning electron microscopy (SEM). Catalytic properties are examined using standard ammonia selective catalytic reduction (NH3-SCR) and ammonia oxidation reactions. In Cu-SAPO-34 samples formed using SSIE, Cu presents both as isolated Cu2+ ions and unreacted CuO. The former is highly active and selective in NH3-SCR, while the latter catalyzes a side reaction; notably, the non-selective oxidation of NH3 above 350 ºC. Using the one-pot method followed by a high-temperature aging treatment, it is possible to form Cu SAPO-34 samples with predominately isolated Cu2+ ions at low Cu loadings. However at much higher Cu loadings, isolated Cu2+ ions that bind weakly with the CHA framework and CuO clusters also form. These Cu moieties are very active in catalyzing non-selective NH3 oxidation above 350 ºC. Low-temperature reaction kinetics indicate that Cu-SAPO-34 samples formed using SSIE have core-shell structures where Cu is enriched in the shell layers; while Cu is more evenly distributed within the one-pot samples. Reaction kinetics also suggest that at low temperatures, the local environment next to Cu2+ ion centers plays little role on the overall catalytic properties. The authors gratefully acknowledge the US Department of Energy (DOE), Energy Efficiency and Renewable Energy, Vehicle Technologies Office for the support of this work. The research described in this paper was performed at the Environmental

  14. Polymer supported sulphanilic acid: A highly efficient and recyclable green heterogeneous catalyst for the construction of 4,5-dihydropyrano[3,2-c]chromenes under solvent-free conditions

    Indian Academy of Sciences (India)

    Jashmin P Patel; Jemin R Avalani; Dipak K Raval

    2013-05-01

    Polystyrene divinylbenzene supported sulphanilic acid was prepared, characterized and tested as an acidic catalyst in multicomponent organic synthesis. This is the first report focusing on the development of one-pot solvent-free synthesis of 4,5- dihydropyrano [3,2-c]chromenes under acidic conditions. It proved to be a versatile catalyst for microwave-assisted synthesis of 4,5-dihydropyrano[3,2-c]chromenes. This methodology is mild, high yielding, green and the catalyst could be easily recycled for several times.

  15. Enzymatic Menthol Production: One-Pot Approach Using Engineered Escherichia coli.

    Science.gov (United States)

    Toogood, Helen S; Ní Cheallaigh, Aisling; Tait, Shirley; Mansell, David J; Jervis, Adrian; Lygidakis, Antonios; Humphreys, Luke; Takano, Eriko; Gardiner, John M; Scrutton, Nigel S

    2015-10-16

    Menthol isomers are high-value monoterpenoid commodity chemicals, produced naturally by mint plants, Mentha spp. Alternative clean biosynthetic routes to these compounds are commercially attractive. Optimization strategies for biocatalytic terpenoid production are mainly focused on metabolic engineering of the biosynthesis pathway within an expression host. We circumvent this bottleneck by combining pathway assembly techniques with classical biocatalysis methods to engineer and optimize cell-free one-pot biotransformation systems and apply this strategy to the mint biosynthesis pathway. Our approach allows optimization of each pathway enzyme and avoidance of monoterpenoid toxicity issues to the host cell. We have developed a one-pot (bio)synthesis of (1R,2S,5R)-(-)-menthol and (1S,2S,5R)-(+)-neomenthol from pulegone, using recombinant Escherichia coli extracts containing the biosynthetic genes for an "ene"-reductase (NtDBR from Nicotiana tabacum) and two menthone dehydrogenases (MMR and MNMR from Mentha piperita). Our modular engineering strategy allowed each step to be optimized to improve the final production level. Moderate to highly pure menthol (79.1%) and neomenthol (89.9%) were obtained when E. coli strains coexpressed NtDBR with only MMR or MNMR, respectively. This one-pot biocatalytic method allows easier optimization of each enzymatic step and easier modular combination of reactions to ultimately generate libraries of pure compounds for use in high-throughput screening. It will be, therefore, a valuable addition to the arsenal of biocatalysis strategies, especially when applied for (semi)-toxic chemical compounds. PMID:26017480

  16. One-pot synthesis of hematite@graphene core@shell nanostructures for superior lithium storage

    Science.gov (United States)

    Chen, Dezhi; Quan, Hongying; Liang, Junfei; Guo, Lin

    2013-09-01

    Novel hematite@graphene composites have been successfully synthesized by a one-pot surfactant governed approach under mild wet-chemical conditions. A series of characterizations including X-ray diffraction (XRD), Raman spectrum, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the hematite nanoparticles with relatively uniform size were encapsulated by graphene layers and were able to form core-shell nanostructures. The electrochemical properties of hematite@graphene core-shell nanostructures as anodes for lithium-ion batteries were evaluated by galvanostatic charge-discharge and AC impedance spectroscopy techniques. The as-prepared hematite@graphene core-shell nanostructures exhibited a high reversible specific capacity of 1040 mA h g-1 at a current density of 200 mA g-1 (0.2 C) after 180 cycles and excellent rate capability and long cycle life. Furthermore, a reversible capacity as high as 500 mA h g-1 was still achieved after 200 cycles even at a high rate of 6 C. The electrochemical test results show that the hematite@graphene composites prepared by the one-pot wet chemical method are promising anode materials for lithium-ion batteries.Novel hematite@graphene composites have been successfully synthesized by a one-pot surfactant governed approach under mild wet-chemical conditions. A series of characterizations including X-ray diffraction (XRD), Raman spectrum, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the hematite nanoparticles with relatively uniform size were encapsulated by graphene layers and were able to form core-shell nanostructures. The electrochemical properties of hematite@graphene core-shell nanostructures as anodes for lithium-ion batteries were evaluated by galvanostatic charge-discharge and AC impedance spectroscopy techniques. The as-prepared hematite@graphene core-shell nanostructures exhibited a high reversible specific capacity of 1040 mA h g-1 at a

  17. One-Pot Synthesis of Tetrahydrobenzo-[b]-pyran Derivatives in Aqueous Media

    Institute of Scientific and Technical Information of China (English)

    JIN,Tong-Shou; WANG,Ai-Qing; ZHANG,Jian-She; LI,Tong-Shuang

    2004-01-01

    @@ In modem organic chemical research, 4H-benzo-[b]-pyran and their derivatives have attracted strong interest due to their useful biological and pharmacological properties. Herein, we report a clean one-pot synthesis of 2-amino-3-cyano-4-aryl-7,7-dimethyl-5-oxo-4H-5,6,7,8-tetrahydro-benzo-[b]-pyrans from aromatic aldehyde, malononitrile and 5,5-dimethyl-1,3-cyclohexadione using hexadecyl trimethyl ammonium bromide (HTMAB) as the catalyst. This method provides several advantages such as high yield, simple work-up procedure and environmental friendliness. All the products were characterized by 1H NMR and IR analyses.

  18. A practical one pot synthesis of novel 2-hydroxy-4-chromanone derivatives from 3-formylchromone

    Indian Academy of Sciences (India)

    Zeba N Siddiqui; Farheen Farooq

    2012-09-01

    A one pot synthesis of 4-chromanone derivatives (5a-j) is described using Zn[(L)(proline)]2 as catalyst in aqueous media. The compounds have been characterized on the basis of elemental and spectral data (IR, 1H NMR and mass). The advantages of this protocol include high yields, mild reaction conditions, environmentally benign and simple operational procedure. The use of water as solvent and Zn[(L)proline]2 as recyclable, non-toxic catalyst make such synthesis a truly green process.

  19. 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.

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

    Science.gov (United States)

    Bernal, M. Mar; Pérez, Emilio M.

    2015-01-01

    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). PMID:25984598

  1. Gold nanoparticles with cyclic phenylazomethines: one-pot synthesis and metal ion sensing.

    Science.gov (United States)

    Shomura, Ryo; Chung, Keum Jee; Iwai, Hideo; Higuchi, Masayoshi

    2011-07-01

    New gold nanoparticles covered with cyclic phenylazomethine (CPA) were obtained by a one-pot synthesis. It is confirmed by XPS that imines of CPA in the nanoparticles (Au-CPA) are partially reduced to amines. The amine part of CPA in Au-CPA is attached to the surfaces of gold nanoparticles, and the imine part works as a redox-active site. A glassy carbon electrode modified with Au-CPA was revealed to work as an electrochemical probe for metal ion sensing.

  2. One-pot synthesis of network supported catalyst using supramolecular gel as template

    Institute of Scientific and Technical Information of China (English)

    Yong Liang; Li Ming Tang; Yu Xia; Kai Chen; Bo Tian Li; Xin Jin

    2010-01-01

    A simple and general strategy is described for preparing network supported catalyst through a one-pot synthetic procedure using supramolecular gel as template. This procedure directly attaches iigand to support during fabricating the support. Using this strategy, supported CuBr/di-(2-picolyl)amine catalyst with U-shaped fibrillar network was prepared and used in atom transfer radical polymerization of methyl methacrylate. XPS and SEM characterization of the catalyst revealed homogeneous distribution of ligand, sufficient reactive sites, adequate mechanical strength and macroporosity. The polymerization results demonstrated high activity and reusability of such catalyst. This strategy might be extended to other supported catalysts used in column reactors.

  3. One-pot Synthesis of Dimethyl Carbonate in the Presence of a Two-component Catalyst

    Institute of Scientific and Technical Information of China (English)

    CHEN Xiu-zhi; HU Chang-wen; GAO Zhi-ming

    2005-01-01

    The one-pot synthesis of dimethyl carbonate (DMC) with co-production of propy-lene carbonate(PC) and propylene glycol(PG) from propylene oxide( PO), carbon dioxide and methanol as the starting materials was investigated.The catalyst adopted here was a mixture of tetrabutyl ammonium bromide and sodium methoxide. It was found that under the reaction conditions of t = 150 ℃, p =3-4 MPa and 2 h, the PO conversion could reach 100%, the DMC,PC and the PG selectivities were 49.7%, 42.7% and 49. 8%, respectively, and the selectivity of by-products was below 10%.

  4. One-pot and two-step synthesis of novel carbonylthioureas and dicarbonyldithioureas derivatives

    Science.gov (United States)

    Banaei, Alireza; Shiran, Jafar Abbasi; Saadat, Afshin; Ardabili, Farnaz Fazlalizadeh; McArdle, Patrick

    2015-11-01

    One-pot, two-step synthesis of several 1-cyclopropanecarbonyl-3-(substituted phenyl)-thioureas and 1-(phenylene-1,4-dione)-3,3‧-(substituted phenyl)-dithioureas have been successfully prepared. The structures of the synthesized compounds were confirmed by elemental analysis, FT-IR spectroscopy and NMR. Also the crystal structure one of these compounds was determined by X-ray crystallography. All synthesized compounds were evaluated for antibacterial activity using Salmonella enterica (SE), Micrococcus luteus (ML), Bacillus subtilis (BS) and Pseudomonas aeruginosa (PS).

  5. One-pot synthesis and characterization of a new, branched polycarbosilane bearing allyl groups

    Institute of Scientific and Technical Information of China (English)

    Tian Hua Huang; Zhao Ju Yu; Xu Min He; Mu He Huang; Li Fu Chen; Hai Ping Xia; Li Tong Zhang

    2007-01-01

    A highly branched polycarbosilane bearing allyl groups has been prepared by a one-pot synthesis with chloromethyltrichlorosilane, chloromethylmethyldichlorosilane and allyl chloride as the starting materials.The resultant polymer, with the approximate formula [SiH1.2(CH)30.71(CH2CH=CH2)0.09CH2]n,has been characterized by 1H, 13C, and 29Si NMR, GPC, TG and elemental analysis.It could be cross-linked thermally at 170℃ in the absence of oxygen.Pyrolysis of the polymer gave a ceramic with a yield of about 70%.

  6. Solvent-free, supersoft and superelastic bottlebrush melts and networks

    Science.gov (United States)

    Daniel, William F. M.; Burdyńska, Joanna; Vatankhah-Varnoosfaderani, Mohammad; Matyjaszewski, Krzysztof; Paturej, Jarosław; Rubinstein, Michael; Dobrynin, Andrey V.; Sheiko, Sergei S.

    2016-02-01

    Polymer gels are the only viable class of synthetic materials with a Young's modulus below 100 kPa conforming to biological applications, yet those gel properties require a solvent fraction. The presence of a solvent can lead to phase separation, evaporation and leakage on deformation, diminishing gel elasticity and eliciting inflammatory responses in any surrounding tissues. Here, we report solvent-free, supersoft and superelastic polymer melts and networks prepared from bottlebrush macromolecules. The brush-like architecture expands the diameter of the polymer chains, diluting their entanglements without markedly increasing stiffness. This adjustable interplay between chain diameter and stiffness makes it possible to tailor the network's elastic modulus and extensibility without the complications associated with a swollen gel. The bottlebrush melts and elastomers exhibit an unprecedented combination of low modulus (~100 Pa), high strain at break (~1,000%), and extraordinary elasticity, properties that are on par with those of designer gels.

  7. Solvent-free microextraction techniques in gas chromatography.

    Science.gov (United States)

    Laaks, Jens; Jochmann, Maik A; Schmidt, Torsten C

    2012-01-01

    Microextraction techniques represent a major part of modern sample preparation in the analysis of organic micropollutants. This article provides a short overview of recent developments in solvent-free microextraction techniques. From the first open-tubular trap techniques in the mid-1980s to recent packed-needle devices, different implementations of in-needle packings for microextraction are discussed with their characteristic benefits, shortcomings and possible sampling modes. Special emphasis is placed on methods providing full automation and solvent exclusion. In this context, in-tube extraction and the needle trap are discussed, with an overview of current research on new sorbent materials, together with the requirements for more efficient method development. PMID:22057686

  8. Solvent-free Michael addition reaction of fluorene with chalcon

    Institute of Scientific and Technical Information of China (English)

    Fu Feng

    2011-01-01

    A series of novel Michael addition products of fluorene to chalcone were obtained in the presence of sodium hydroxide under solvent-free condition. The advantages of this procedure were mild reaction conditions, simple protocol, and high yields. The structures of the products were characterized by IR, 1H NMR, MS and X-ray diffraction. The crystal of the new compound 3 h is y= 64.2440(10)°, V = 2.4137(3) nm3, Z= 4, Dc=1.220 g/cm3, μ = 0.286 mm-1, F(000) = 920, R = 0.0656 and wR = 0.1554 for 5664 observed reflection with I > 2σ(I).

  9. Solvent-free Synthesis of Thiohydantoin Derivatives with Microwave Activation

    Institute of Scientific and Technical Information of China (English)

    LI Jian-ping; MA Chun-ming; QU Gui-rong

    2004-01-01

    The application of microwave techniques for chemical synthesis has attached considerable interests in recent years because of their enhanced selectivity, reduced reaction time ,easier work-up procedure. The synthesis of thiohydantoin derivatives is useful because they display a wide range of biological activities, including anticonvulsant1, antitumor2, antinociceptive3,thyroxine ingibitory properties4, as well as herbicidal and fungicidal reagents5. Recent studies have shown that some used as synthetic precursor of the marine natural product dispacamide6, and some used to synthesis novel optically active poly(amide-imide)s7. Therefore, many methods of synthesis of thiohydantoins have been explored8~10. Generally, these reactions were carried out in solution and using volatile and poisonous solvent, with long reaction time.In order to overcome the disadvantages discussed above, avoid the use of a solvent and synthesize these valuable compounds rapidly and efficiently, we investigated a new way---solvent-free synthesis using a microwave oven.In this paper, a new and rapid solvent-free synthesis of thiohydantoins with microwave activation was studied. It was found that the addition reaction of aryl isothiocyanates and amino acid in the presence of sodium hydroxide and the cyclizative condensation of adduct in the presence of sodium hydrogen sulphate in a microwave oven takes place quickly.By this new method, twelve thiohydantoins have been synthesized in excellent yield(83~91%).This method has significant advantages such as operational simplicity, shorter reaction time, higher yields and environmental acceptability. The structures of the products were characterized by IR, MS,1H NMR, 13C NMR and elemental analysis. And more detailed work about the application of the thiohydantoins in analytical chemistry and physiological activity is in progress in our laboratory.

  10. 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.

  11. Ag(I)-triggered one-pot synthesis of Ag nanoparticles onto natural nanorods as a multifunctional nanocomposite for efficient catalysis and adsorption.

    Science.gov (United States)

    Tian, Guangyan; Wang, Wenbo; Mu, Bin; Kang, Yuru; Wang, Aiqin

    2016-07-01

    A multifunctional palygorskite/polyaniline/Ag nanoparticles (PAL/PANI/AgNPs) nanocomposite was prepared at room temperature using a simple one-pot in-situ polymerization reaction of aniline monomers triggered by Ag(I) on the surface of natural PAL nanorods. Ag(I) served as both the oxidant and the precursor of the AgNPs, which initiated the polymerization of aniline monomers on PAL nanorods while simultaneously being reduced to form Ag(0) nanoparticles (AgNPs). The in-situ formed AgNPs were evenly distributed on the surface of the PAL nanorods because the interfacial effect of PAL prevents their aggregation. The density and size of the AgNPs and the catalytic activity of the nanocomposites could be controlled by altering the molar ratio of aniline to Ag(I). The performance evaluation revealed that the nanocomposites could be used as highly active catalysts, which rapidly catalyzed the reduction of 4-nitrophenol (4-NP) within 2min and Congo red (CR) within 10min. The nanocomposites are also an effective adsorbent for H2PO4(-) able to remove 99.40% of H2PO4(-) (only 61.77% for raw PAL) from a solution with an initial concentration of 50mg/L. This multifunctional nanocomposite synthesized by a simple one-pot approach is a promising material for environmental applications. PMID:27054770

  12. Microwave Assisted Solvent Free Synthesis of Azomethines from Aryl Aldehydes on Melamin Formaldehyde as Solid Support

    OpenAIRE

    Ramin Rezaei; Mohammadi, Mohammad K; Tahereh Ranjbar

    2011-01-01

    Various aryl aldehydes underwent prompt one pot conversion into the corresponding azomethines in high yields by reacting with hydroxylamine hydrochloride supported on melamine formaldehyde under microwave irradiation.

  13. 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)

  14. 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.

  15. 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.

  16. One-Pot Synthesis of Cu(II Complex with Partially Oxidized TTF Moieties

    Directory of Open Access Journals (Sweden)

    Hiroki Oshio

    2012-07-01

    Full Text Available The one-pot synthesis of a Cu(II complex with partially oxidized tetrathiafulvalene (TTF moieties in its capping MT-Hsae-TTF ligands, [CuII(MT-sae-TTF2] [CuICl2] was realized by the simultaneous occurrence of Cu(II complexation and CuIICl2 mediated oxidation of TTF moieties. The crystal structure was composed of one-dimensional columns formed by partially oxidized TTF moieties and thus the cation radical salt showed relatively high electrical conductivity. Tight binding band structure calculations indicated the existence of a Peierls gap due to the tetramerization of the TTF moieties in the one-dimensional stacking column at room temperature, which is consistent with the semiconducting behavior of this salt.

  17. Simple one-pot synthesis of thioureas from amine, carbon disulfide and oxidants in water

    Directory of Open Access Journals (Sweden)

    Milosavljević Milutin M.

    2016-01-01

    Full Text Available The present study reports the new facile methodology for synthesis of symmetrical and asymmetrical thioureas by an one-pot reaction of amine, carbon disulfide and oxidants: hydrogen peroxide, ethylenediamine tetraacetic acid (EDTA/sodium percarbonate system or air. The structures of the synthesized compounds were confirmed by IR, 1H and 13C NMR and MS methods. Reaction mechanism has been proposed on the basis of reaction intermediate isolation and their structure determination. The synthetic benefits of the presented methods is reflected in the operational simplicity, mild reaction conditions, short reaction times, recycling of solvent, high purity and yield of products, absence of dangerous by-products and technological applicability at industrial scale. Considering commercial importance of the thioureas, it can be emphasized that implementation of the optimal synthesis of thiourea, based on presented methods, at industrial level of production would provide concurrent alternative to existing technologies in use. [Projekat Ministarstva nauke Republike Srbije, br. 172013

  18. A one-pot reaction to synthesize two types of fluorescent materials containing benzothiazolyl moiety.

    Science.gov (United States)

    Yu, Tianzhi; Zhang, Chengcheng; Zhao, Yuling; Chai, Haifang; Fan, Duowang; Ma, Ying; Yao, Shanglei; Li, Wentao

    2013-05-01

    Two different types of fluorescent materials containing benzothiazolyl moiety, 2-(benzothiazol-2-yl)phenol derivatives and 3-(benzothiazol-2-yl)coumarin derivatives, were synthesized synchronously using ethyl cyanoacetate, appropriate aromatic aldehyde and 2-aminothiophenol as the starting materials under the catalysis of benzoic acid by one-pot reaction. This method has the advantages of mild reaction conditions, easy processing and low waste. All synthesized compounds were characterized by elemental analysis, IR, (1)H NMR spectra. The structures of 2-(benzothiazol-2-yl)phenol derivatives, 2-(benzothiazol-2-yl)phenol (BTP) and 2-(benzothiazol-2-yl)naphthol (BTN), were determined by X-ray single crystal analysis. The UV-vis absorption and photoluminescence spectra of all synthesized compounds were investigated. The 2-(benzothiazol-2-yl)phenol derivatives exhibit bright green emissions and 3-(benzothiazol-2-yl)coumarin derivatives emit bright blue light in solutions.

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

    International Nuclear Information System (INIS)

    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

  20. One-pot synthesis of PVA-capped silver nanoparticles their characterization and biomedical application

    International Nuclear Information System (INIS)

    The rapid one-pot synthesis of silver nanoparticles (SNPs) at room temperature by using hydrazine hydrate as reducing agent and polyvinyl alcohol as stabilizing agent is reported. The SNPs were characterized with UV-visible (UV-Vis) spectroscopy, x-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). The synthesized silver nanoparticle shows surface plasmon resonance at 410 nm. The XRD reveals face-centered cubic (FCC) structure of SNPs. FE-SEM, AFM and TEM show that nanoparticles have spherical morphology with diameters in the range of 10–60 nm. The antimicrobial activity of synthesized hybrid material against strains of four different bacteria (Bacillus cereus, Escherichia coli, Staphylococus aureus, Proteus vulgaris), that are commonly found in hospitals has been studied. The results indicate that such particles have potential applications in biotechnology and biomedical science

  1. A facile one-pot method to synthesize ultrasmall core-shell superparamagnetic and upconversion nanoparticles.

    Science.gov (United States)

    Cheng, Qian; Guo, Hongxuan; Li, Yu; Liu, Shouxin; Sui, Jiehe; Cai, Wei

    2016-08-01

    Ultrasmall core-shell Fe3O4@NaYF4:Yb(3+)/Er(3+) nanoparticles with bifunctional properties have been successfully synthesized via one pot thermolysis method using oleylamine as both solvent and stabilizer. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), upconversion (UC) luminescence spectra and the physical properties measurement system (PPMS) were used to characterize the resulting samples. The synthesized samples have uniform morphology with a mean size of 14.5nm and excellent dispersibility. Moreover, these nanoparticles exhibit superparamagnetic behaviour with saturation magnetization of 8.45emμ/g and efficient up-conversion emission with a two-photon induced process when excited by a 980nm laser. These results suggest that the synthesized ultrasmall bifunctional nanoparticles may find many biomedical applications, such as clinical diagnosis and treatment of cancers. PMID:27135942

  2. One-pot synthesis of PVA-capped silver nanoparticles their characterization and biomedical application

    Science.gov (United States)

    Patil, Rupali S.; Kokate, Mangesh R.; Jambhale, Chitra L.; Pawar, Sambhaji M.; Han, Sung H.; Kolekar, Sanjay S.

    2012-03-01

    The rapid one-pot synthesis of silver nanoparticles (SNPs) at room temperature by using hydrazine hydrate as reducing agent and polyvinyl alcohol as stabilizing agent is reported. The SNPs were characterized with UV-visible (UV-Vis) spectroscopy, x-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). The synthesized silver nanoparticle shows surface plasmon resonance at 410 nm. The XRD reveals face-centered cubic (FCC) structure of SNPs. FE-SEM, AFM and TEM show that nanoparticles have spherical morphology with diameters in the range of 10-60 nm. The antimicrobial activity of synthesized hybrid material against strains of four different bacteria (Bacillus cereus, Escherichia coli, Staphylococus aureus, Proteus vulgaris), that are commonly found in hospitals has been studied. The results indicate that such particles have potential applications in biotechnology and biomedical science.

  3. One-pot microbial synthesis of 2'-deoxyribonucleoside from glucose, acetaldehyde, and a nucleobase.

    Science.gov (United States)

    Horinouchi, Nobuyuki; Ogawa, Jun; Kawano, Takako; Sakai, Takafumi; Saito, Kyota; Matsumoto, Seiichiro; Sasaki, Mie; Mikami, Yoichi; Shimizu, Sakayu

    2006-06-01

    A one-pot enzymatic synthesis of 2'-deoxyribonucleoside from glucose, acetaldehyde, and a nucleobase was established. Glycolysis by baker's yeast (Saccharomyces cerevisiae) generated ATP which was used to produce D: -glyceraldehyde 3-phosphate production from glucose via fructose 1,6-diphosphate. The D: -glyceraldehyde 3-phosphate produced was transformed to 2'-deoxyribonucleoside via 2-deoxyribose 5-phosphate and then 2-deoxyribose 1-phosphate in the presence of acetaldehyde and a nucleobase by deoxyriboaldolase, phosphopentomutase expressed in Escherichia coli, and a commercial nucleoside phosphorylase. About 33 mM 2'-deoxyinosine was produced from 600 mM glucose, 333 mM acetaldehyde and 100 mM adenine in 24 h. 2'-Deoxyinosine was produced from adenine due to the adenosine deaminase activity of E. coli transformants.

  4. A facile one-pot method to Au–SnO{sub 2}-graphene ternary hybrid

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Diou, E-mail: xudiou@sina.com [Department of Agriculture, Jilin University, Changchun 130062 (China); Li, Xiaotian [College of Materials Science and Engineering, Jilin University, Changchun 130012 (China); Zhang, Dawei [Department of Agriculture, Jilin University, Changchun 130062 (China)

    2014-11-15

    In this article, we propose a facile one-pot route for synthesizing Au–SnO{sub 2}-graphene ternary hybrid. In the system, SnCl{sub 2} not only as the precursor of SnO{sub 2}, but also is employed as reducing agent for the effective reduction of both GO and HAuCl{sub 4} to graphene and Au nanoparticles, respectively. The obtained Au–SnO{sub 2}-graphene hybrid materials are characterized by atomic force microscopy, transmission electron microscopy, X-ray diffraction, Raman spectrum, X-ray photo-electron spectroscopy, and thermal gravimetric analysis. It is found that the content of Au nanoparticles decorated on the surface of graphene can be simply adjusted by changing the amount of HAuCl{sub 4} used in the synthesis process.

  5. Solvent-free enzymatic production of high quality cetyl esters.

    Science.gov (United States)

    Serrano-Arnaldos, Mar; Máximo-Martín, María Fuensanta; Montiel-Morte, María Claudia; Ortega-Requena, Salvadora; Gómez-Gómez, Elisa; Bastida-Rodríguez, Josefa

    2016-04-01

    A solvent-free biocatalytic process for the synthesis of high quality cetyl laurate, myristate, palmitate and stearate has been optimized. This enzymatic procedure follows the fundamental principles of the Green Chemistry and lead to sustainable products, which can be labeled as natural and conform to the principal requirements for its use in high value-added goods. The four esters selected are the main components of spermaceti, a mixture of waxes very appreciated in cosmetic and pharmacy because of its physical properties and emolliency, which was formerly extracted from the head of the sperm whales. In this paper, the influence of the amount of biocatalyst, the commercially available Novozym(®) 435, and the temperature were studied in an open-air batch reactor before carrying out the synthesis in a high performance vacuum reactor with dry nitrogen input to shift the equilibrium towards product formation. Under optimal conditions, conversion was higher than 98.5 %. The characterization of the enzymatic cetyl esters puts in evidence that these are ultra-pure compounds, which have similar properties to the ones obtained through the conventional industrial processes with the extra benefit of being environmentally friendly. PMID:26801670

  6. Solvent-free covalent functionalization of nanodiamond with amines

    International Nuclear Information System (INIS)

    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.

  7. [{sup 11}C]GR103545: novel one-pot radiosynthesis with high specific activity

    Energy Technology Data Exchange (ETDEWEB)

    Nabulsi, Nabeel B., E-mail: nabeel.nabulsi@yale.ed [Department of Diagnostic Radiology, PET Center, Yale School of Medicine, PO Box 208048, New Haven, CT 06520-8048 (United States); Zheng Mingqiang; Ropchan, Jim; Labaree, David; Ding Yushin [Department of Diagnostic Radiology, PET Center, Yale School of Medicine, PO Box 208048, New Haven, CT 06520-8048 (United States); Blumberg, Laura [Pfizer Global R and D, Groton, CT 06340 (United States); Huang Yiyun [Department of Diagnostic Radiology, PET Center, Yale School of Medicine, PO Box 208048, New Haven, CT 06520-8048 (United States)

    2011-02-15

    Introduction: GR103545 is a potent and selective kappa-opioid receptor agonist. Previous studies in non-human primates demonstrated favorable properties of [{sup 11}C]GR103545 as a positron emission tomography tracer for in vivo imaging of cerebral kappa-opioid receptor. Nonetheless, advancement of [{sup 11}C]GR103545 to imaging studies in humans was hampered by difficulties of its multiple-step radiosynthesis, which produces a final product with low specific activity (SA), which in turn could induce undesirable physiological side effects resulting from the mass associated with an injected amount of radioactivity. We report herein an alternative radiosynthesis of [{sup 11}C]GR103545 with higher SA and radiochemical yields. Methods: The TRACERLab FXC automated synthesis module was used to carry out the two-step, one-pot procedure. In the first step, the desmethoxycarbonyl precursor was converted to the carbamic acid intermediate desmethyl-GR103545 via transcarboxylation with the zwitterionic carbamic complex, 1,8-diazabicyclo[5.4.0]undec-7-ene-carbon dioxide, in the presence and/or absence of cesium carbonate and tetrabutylammonium triflate. In the second step, the intermediate was radiolabeled at the carboxyl oxygen with [{sup 11}C]methyl trifluoromethanesulfonate to give [{sup 11}C]GR103545. Results: This novel synthesis produced [{sup 11}C]GR103545 with {>=}90% chemical and radiochemical purities and an SA of 290.45{+-}99.9 MBq/nmol at the end of synthesis (n=26). Injectable radioactivity was 1961{+-}814 GBq/{mu}mol with 43 min of average synthesis time from the end of beam. Conclusion: We have developed a practical one-pot method for the routine production of [{sup 11}C]GR103545 with reliably high SA and radiochemical yield, thus allowing the advancement of this radiotracer to imaging applications in humans.

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

    Directory of Open Access Journals (Sweden)

    Christian Leisner

    Full Text Available 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 of vaccines and adoptive immune therapy. Peptide-MHC tetramers have become important reagents for detection and enumeration of specific CTL's. Conventional peptide-MHC-tetramer production involves recombinant MHC production, in vitro refolding, biotinylation and tetramerization; each step followed by various biochemical steps such as chromatographic purification, concentration etc. Such cumbersome production protocols have limited dissemination and restricted availability of peptide-MHC tetramers effectively precluding large-scale screening strategies involving many different peptide-MHC tetramers. METHODOLOGY/PRINCIPAL FINDINGS: We have developed an approach whereby any given tetramer specificity can be produced within 2 days with very limited effort and hands-on time. The strategy is based on the isolation of correctly oxidized, in vivo biotinylated recombinant MHC I heavy chain (HC. Such biotinylated MHC I HC 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, and demonstrated specific T cell straining comparable to a commercially available MHC-tetramer. Here, seven peptide-MHC tetramers representing four different human MHC (HLA class I proteins have been generated. The technique should be readily extendable to any binding peptide and pre-biotinylated MHC (at this time we have over 40 different pre-biotinylated HLA proteins. It is simple, robust, and versatile technique with a very broad application

  9. Tuneable light-emitting carbon-dot/polymer flexible films prepared through one-pot synthesis

    Science.gov (United States)

    Bhunia, Susanta Kumar; Nandi, Sukhendu; Shikler, Rafi; Jelinek, Raz

    2016-02-01

    Development of efficient, inexpensive, and environmentally-friendly light emitters, particularly devices that produce white light, have drawn intense interest due to diverse applications in the lighting industry, photonics, solar energy, and others. We present a simple strategy for the fabrication of flexible transparent films exhibiting tuneable light emission through one-pot synthesis of polymer matrixes with embedded carbon dots assembled in situ. Importantly, different luminescence colours were produced simply by preparing C-dot/polymer films using carbon precursors that yielded C-dots exhibiting distinct fluorescence emission profiles. Furthermore, mixtures of C-dot precursors could be also employed for fabricating films exhibiting different colours. In particular, we successfully produced films emitting white light with attractive properties (i.e. ``warm'' white light with a high colour rendering index) - a highly sought after goal in optical technologies.Development of efficient, inexpensive, and environmentally-friendly light emitters, particularly devices that produce white light, have drawn intense interest due to diverse applications in the lighting industry, photonics, solar energy, and others. We present a simple strategy for the fabrication of flexible transparent films exhibiting tuneable light emission through one-pot synthesis of polymer matrixes with embedded carbon dots assembled in situ. Importantly, different luminescence colours were produced simply by preparing C-dot/polymer films using carbon precursors that yielded C-dots exhibiting distinct fluorescence emission profiles. Furthermore, mixtures of C-dot precursors could be also employed for fabricating films exhibiting different colours. In particular, we successfully produced films emitting white light with attractive properties (i.e. ``warm'' white light with a high colour rendering index) - a highly sought after goal in optical technologies. Electronic supplementary information (ESI

  10. A Novel One-Pot and One-Step Microwave-Assisted Cyclization-Methylation Reaction of Amino Alcohols and Acetylated Derivatives with Dimethyl Carbonate and TBAC

    Science.gov (United States)

    Ochoa-Terán, Adrián; Guerrero, Leticia; Rivero, Ignacio A.

    2014-01-01

    A simple and efficient microwave-assisted methodology for the synthesis of 4-substituted-3-methyl-1,3-oxazolidin-2-ones from amino alcohols catalyzed by a ionic liquid was developed. This novel one-pot and one-step cyclization-methylation reaction represents an easier and faster method than any other reported protocols that can be used to obtain the desired products in good yields and high purity. Applying microwave irradiation at 130°C in the presence of TBAC, dimethyl carbonate acts simultaneously as carbonylating and methylating agent and surprisingly promotes an in situ basic trans esterification when a N-acetylated amino alcohol is used as starting material. Furthermore, dimethyl carbonate worked better than diethyl carbonate in performing this reaction. PMID:25692177

  11. A novel one-pot and one-step microwave-assisted cyclization-methylation reaction of amino alcohols and acetylated derivatives with dimethyl carbonate and TBAC.

    Science.gov (United States)

    Ochoa-Terán, Adrián; Guerrero, Leticia; Rivero, Ignacio A

    2014-01-01

    A simple and efficient microwave-assisted methodology for the synthesis of 4-substituted-3-methyl-1,3-oxazolidin-2-ones from amino alcohols catalyzed by a ionic liquid was developed. This novel one-pot and one-step cyclization-methylation reaction represents an easier and faster method than any other reported protocols that can be used to obtain the desired products in good yields and high purity. Applying microwave irradiation at 130°C in the presence of TBAC, dimethyl carbonate acts simultaneously as carbonylating and methylating agent and surprisingly promotes an in situ basic trans esterification when a N-acetylated amino alcohol is used as starting material. Furthermore, dimethyl carbonate worked better than diethyl carbonate in performing this reaction. PMID:25692177

  12. A Novel One-Pot and One-Step Microwave-Assisted Cyclization-Methylation Reaction of Amino Alcohols and Acetylated Derivatives with Dimethyl Carbonate and TBAC

    Directory of Open Access Journals (Sweden)

    Adrián Ochoa-Terán

    2014-01-01

    Full Text Available A simple and efficient microwave-assisted methodology for the synthesis of 4-substituted-3-methyl-1,3-oxazolidin-2-ones from amino alcohols catalyzed by a ionic liquid was developed. This novel one-pot and one-step cyclization-methylation reaction represents an easier and faster method than any other reported protocols that can be used to obtain the desired products in good yields and high purity. Applying microwave irradiation at 130°C in the presence of TBAC, dimethyl carbonate acts simultaneously as carbonylating and methylating agent and surprisingly promotes an in situ basic trans esterification when a N-acetylated amino alcohol is used as starting material. Furthermore, dimethyl carbonate worked better than diethyl carbonate in performing this reaction.

  13. Regioselective ring opening of epoxides using NH4SCN/silica sulfuric acid: An efficient approach for the synthesis of β-hydroxy thiocyanate under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Ali R. Kiasat; Maryam Zayadi; Mehdi Fallah Mehrjardi

    2008-01-01

    Silica sulfuric acid was developed as a stable and efficient heterogeneous catalyst in organic synthesis. This solid acid catalyzed the regioselective ring opening of epoxides by thiocyanate anion to give thiocyanohydrins as key intermediates in agricultural and pharmaceutical chemistry in high yields under solvent-free conditions.

  14. An insight on acyl migration in solvent-free ethanolysis of model triglycerides using Novozym 435.

    Science.gov (United States)

    Sánchez, Daniel Alberto; Tonetto, Gabriela Marta; Ferreira, María Luján

    2016-02-20

    In this work, the ethanolysis of triglycerides catalyzed by immobilized lipase was studied, focusing on the secondary reaction of acyl migration. The catalytic tests were performed in a solvent-free reaction medium using Novozym 435 as biocatalyst. The selected experimental variables were biocatalyst loading (5-20mg), reaction time (30-90min), and chain length of the fatty acids in triglycerides with and without unsaturation (short (triacetin), medium (tricaprylin) and long (tripalmitin/triolein)). The formation of 2-monoglyceride by ethanolysis of triglycerides was favored by long reaction times and large biocatalyst loading with saturated short- to medium-chain triglycerides. In the case of long-chain triglycerides, the formation of this monoglyceride was widely limited by acyl migration. In turn, acyl migration increased the yield of ethyl esters and minimized the content of monoglycerides and diglycerides. Thus, the enzymatic synthesis of biodiesel was favored by long-chain triglycerides (which favor the acyl migration), long reaction times and large biocatalyst loading. The conversion of acylglycerides made from long-chain fatty acids with unsaturation was relatively low due to limitations in their access to the active site of the lipase. PMID:26795690

  15. Lipozyme TL IM as Catalyst for the Synthesis of Eugenyl Acetate in Solvent-Free Acetylation.

    Science.gov (United States)

    Silva, María José A; Loss, Raquel A; Laroque, Denise A; Lerin, Lindomar A; Pereira, Gabriela N; Thon, Élise; Oliveira, J Vladimir; Ninow, Jorge L; Hense, Haiko; Oliveira, Débora

    2015-06-01

    The ability of commercial immobilized lipase from Thermomyces lanuginosus (Lipozyme TL IM) to catalyze the acetylation of essential clove oil with acetic anhydride in a solvent-free system was studied, and the antimicrobial activity of the ester formed was evaluated as well. Experimental design based on two variables (eugenol to acetic anhydride molar ratio and temperature) was employed to evaluate the experimental conditions of eugenyl acetate ester production. The maximum conversion yield (92.86 %) was obtained using Lipozyme TL IM (5 wt%, based on the total amount of substrates), with eugenol to acetic anhydride molar ratio of 1:5 at 70 °C. The chemical structure of the eugenyl acetate ester obtained at the optimized condition, and purified, was confirmed by the proton nuclear magnetic resonance ((1)H-NMR) analysis. The antimicrobial activity of eugenyl acetate ester was proven effective on Gram-positive and Gram-negative bacteria, with means of 16.62 and 17.55 mm of inhibition halo. PMID:25875787

  16. Isothermal DNA origami folding: avoiding denaturing conditions for one-pot, hybrid-component annealing

    Science.gov (United States)

    Kopielski, Andreas; Schneider, Anne; Csáki, Andrea; Fritzsche, Wolfgang

    2015-01-01

    The DNA origami technique offers great potential for nanotechnology. Using biomolecular self-assembly, defined 2D and 3D nanoscale DNA structures can be realized. DNA origami allows the positioning of proteins, fluorophores or nanoparticles with an accuracy of a few nanometers and enables thereby novel nanoscale devices. Origami assembly usually includes a thermal denaturation step at 90 °C. Additional components used for nanoscale assembly (such as proteins) are often thermosensitive, and possibly damaged by such harsh conditions. They have therefore to be attached in an extra second step to avoid defects. To enable a streamlined one-step nanoscale synthesis - a so called one-pot folding - an adaptation of the folding procedures is required. Here we present a thermal optimization of this process for a 2D DNA rectangle-shaped origami resulting in an isothermal assembly protocol below 60 °C without thermal denaturation. Moreover, a room temperature protocol is presented using the chemical additive betaine, which is biocompatible in contrast to chemical denaturing approaches reported previously.The DNA origami technique offers great potential for nanotechnology. Using biomolecular self-assembly, defined 2D and 3D nanoscale DNA structures can be realized. DNA origami allows the positioning of proteins, fluorophores or nanoparticles with an accuracy of a few nanometers and enables thereby novel nanoscale devices. Origami assembly usually includes a thermal denaturation step at 90 °C. Additional components used for nanoscale assembly (such as proteins) are often thermosensitive, and possibly damaged by such harsh conditions. They have therefore to be attached in an extra second step to avoid defects. To enable a streamlined one-step nanoscale synthesis - a so called one-pot folding - an adaptation of the folding procedures is required. Here we present a thermal optimization of this process for a 2D DNA rectangle-shaped origami resulting in an isothermal assembly

  17. 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 fluoropo

  18. Potassium dihydrogen phosphate catalyzed one-pot synthesis of 2,4,5-triaryl-1H-imidazoles

    Institute of Scientific and Technical Information of China (English)

    Ratnadeep; S.Joshi; Priyanka; G.Mandhane; Mohammad; U.Shaikh; Rajesh; P.Kale; Charansingh; H.Gill

    2010-01-01

    A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate(KH_2PO_4) under mild reaction conditions to afford the corresponding trisubstituted imidazole in excellent yields.The method for synthesis of product,the reaction mixture was reflux in ethanol for 40-90 min.The present method is simple,efficient,and cost-effective.

  19. One pot synthesis, structural and spectral analysis of some symmetrical curcumin analogues catalyzed by calcium oxide under microwave irradiation

    Science.gov (United States)

    Elavarasan, S.; Bhakiaraj, D.; Chellakili, B.; Elavarasan, T.; Gopalakrishnan, M.

    2012-11-01

    A series of sixteen number of curcumin analogues have been synthesized under microwave irradiation using calcium oxide as a catalyst. The synthesized compounds have been characterized using FT-IR, MS, elemental analysis, 1H and 13C NMR spectroscopic techniques. The UV-Vis absorption studies for these compounds have been studied in order to provide the electronic transitions taking place in the molecule. When compared to the curcumin ((1E,4Z,6E)-5-hydroxy-1,7-bis(4-hydroxy-3-methoxyphenyl)hepta-1,4,6-trien-3-one), the absorption maxima, λmax for all the synthesized curcumin analogues with a variety of substituents gets blue shifted i.e., hypsochromic shift was observed. This shift may be assigned to the change of dipole moment within the solvated molecule. Theoretical calculations regarding the optimization of the synthesized molecules, electronic properties like highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) and mapped electron density surface diagrams were done. The geometrical energy, dipole moments and heat of formation values have also been calculated using the ArgusLab package by AM1 semi-empirical method.

  20. Eco-friendly one-pot synthesis of acetals and ketals by heterogeneously catalyzed liquid-solid phase reaction

    Institute of Scientific and Technical Information of China (English)

    YANG Shuijin; WANG Min; LIANG Yongguang; SUN Jutang

    2006-01-01

    Twelve classes of acetals and ketals were synthesized from aldehyde/ketone and glycol using TiSiWl2O40/TiO2 as a novel eco-friendly catalyst. The physical characterizations were carried out by TG/DTA, FT-IR, XRD, and 1H NMR spectra. The results indicated that the catalyst showed excellent catalytic activity for the condensation reactions. The yield of 12classes of acetals and ketals reached 56.3%-96.3% under the typical reaction conditions (the molar ratio of aldehyde/ketone ture was 80-116℃). The catalyst was easily recovered and reused to give almost the same yield of the product as that given by fresh TiSiW12O40/TiO2.

  1. An environmentally benign one pot synthesis of substituted quinolines catalysed by fluoroboric acid based ionic liquid

    Indian Academy of Sciences (India)

    A Rajendran; C Karthikeyan; K Rajathi; D Ragupathy

    2012-07-01

    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 by reaction of substituted anilines with -ketoester at 60°C in ethanol using an ionic liquid [Et3NH]+[BF4]−as catalyst. All the reactions gave products with high degree of purity and excellent yield (78-93%) within the shorter span of time (20-65 min) than those reactions with conventional methods. The screening of solvents as well as the reuse of ionic liquid has been evaluated. The structure of the products has been elucidated by spectral and analytical data. The present scope and potential economic impact of the reaction are demonstrated by the synthesis of substituted quinolines. Remaining challenges and future perspectives of the new transformation are discussed.

  2. Efficient one-pot synthesis of monodisperse alkyl-terminated colloidal germanium nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Carolan, Darragh, E-mail: darragh.carolan@tyndall.ie; Doyle, Hugh, E-mail: hugh.doyle@tyndall.ie [University College Cork, Tyndall National Institute (Ireland)

    2014-12-15

    An efficient one-pot method for fabricating alkyl-capped germanium nanocrystals (Ge NCs) is reported. Ge NCs with a size of 3.9 ± 0.5 nm, are formed by co-reduction of germanium tetrachloride in the presence of n-butyltrichlorogermane, producing NCs with butyl-terminated surfaces. The advantage of this method is that it allows rapid synthesis and functionalisation of NCs with minimal post-synthetic purification requirements. TEM imaging showed that the Ge NCs are monodisperse and highly crystalline, while EDX and SAED confirmed the chemical identity and crystal phase of the NCs. FTIR and XPS confirmed that the Ge NCs were well passivated, with some oxidation of the nanocrystal surface. Optical spectroscopy of the NCs showed a strong absorbance in the UV region and an excitation wavelength dependent photoluminescence in the UV/violet. Time resolved photoluminescence measurements showed the presence of two nanosecond lifetime components, consistent with recombination of photogenerated excitons at low lying energy states present at the nanocrystal surface. Photoluminescence quantum yields were determined to be 37 %, one of the highest values reported for organically terminated Ge NCs.

  3. Efficient One-Pot Synthesis of 5-Chloromethylfurfural (CMF from Carbohydrates in Mild Biphasic Systems

    Directory of Open Access Journals (Sweden)

    Dimitris S. Argyropoulos

    2013-07-01

    Full Text Available 5-Halomethylfurfurals can be considered as platform chemicals of high reactivity making them useful for the preparation of a variety of important compounds. In this study, a one-pot route for the conversion of carbohydrates into 5-chloromethylfurfural (CMF in a simple and efficient (HCl-H3PO4/CHCl3 biphasic system has been investigated. Monosaccharides such as D-fructose, D-glucose and sorbose, disaccharides such as sucrose and cellobiose and polysaccharides such as cellulose were successfully converted into CMF in satisfactory yields under mild conditions. Our data shows that when using D-fructose the optimum yield of CMF was about 47%. This understanding allowed us to extent our work to biomaterials, such as wood powder and wood pulps with yields of CMF obtained being comparable to those seen with some of the enumerated mono and disaccharides. Overall, the proposed (HCl-H3PO4/CHCl3 optimized biphasic system provides a simple, mild, and cost-effective means to prepare CMF from renewable resources.

  4. 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.

  5. Polyacrylamide–metal nanocomposites: one-pot synthesis, antibacterial properties, and thermal stability

    International Nuclear Information System (INIS)

    The incorporation of inorganic nanoparticles into polymers is a hot research spot, since it endows the nanocomposites with new or improved properties by exploiting synergistic effects. Here we report a facile one-pot synthesis of polyacrylamide (PAM)–metal (M = Au, Ag, or Pd) nanocomposites in ethylene glycol (EG). The simultaneous polymerization of the acylamide (AM) monomer and formation of metal nanoparticles lead to a homogeneous distribution of metal nanoparticles in the PAM matrix. The sizes of Au, Ag, and Pd nanoparticles are 55.50 ± 10.6, 14.15 ± 2.57, and 7.74 ± 1.82 nm, respectively. The reaction system only includes EG, AM monomer, and corresponding metal salt. EG acts as both the solvent and the reducing reagent. Also, no initiator for AM polymerization and no surfactant for stabilization of metal nanoparticles are used. Furthermore, this simple synthetic route does not rely on any special or expensive equipment, thus can be exploited to the synthesis of similar polymer–inorganic nanocomposites. Compared to PAM, the PAM–metal nanocomposites showed enhanced thermal stability and antibacterial properties

  6. Polyacrylamide-metal nanocomposites: one-pot synthesis, antibacterial properties, and thermal stability

    Energy Technology Data Exchange (ETDEWEB)

    Li, Cuiyan [Uppsala University, Department of Chemistry - Angstroem Laboratory (Sweden); Cai, Yanling [Uppsala University, Division of Nanotechnology and Functional Materials, Angstroem Laboratory (Sweden); Zhu, Yihua [East China University of Science and Technology, Key Laboratory for Ultrafine Materials of Ministry of Education (China); Ma, Mingguo [Beijing Forestry University, Institute of Biomass Chemistry and Technology, College of Materials Science and Technology (China); Zheng, Wei [University of Wisconsin-Stout, Engineering and Technology Department (United States); Zhu, Jiefang, E-mail: jiefang.zhu@kemi.uu.se [Uppsala University, Department of Chemistry - Angstroem Laboratory (Sweden)

    2013-09-15

    The incorporation of inorganic nanoparticles into polymers is a hot research spot, since it endows the nanocomposites with new or improved properties by exploiting synergistic effects. Here we report a facile one-pot synthesis of polyacrylamide (PAM)-metal (M = Au, Ag, or Pd) nanocomposites in ethylene glycol (EG). The simultaneous polymerization of the acylamide (AM) monomer and formation of metal nanoparticles lead to a homogeneous distribution of metal nanoparticles in the PAM matrix. The sizes of Au, Ag, and Pd nanoparticles are 55.50 {+-} 10.6, 14.15 {+-} 2.57, and 7.74 {+-} 1.82 nm, respectively. The reaction system only includes EG, AM monomer, and corresponding metal salt. EG acts as both the solvent and the reducing reagent. Also, no initiator for AM polymerization and no surfactant for stabilization of metal nanoparticles are used. Furthermore, this simple synthetic route does not rely on any special or expensive equipment, thus can be exploited to the synthesis of similar polymer-inorganic nanocomposites. Compared to PAM, the PAM-metal nanocomposites showed enhanced thermal stability and antibacterial properties.

  7. 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.

  8. One-pot conversions of raffinose into furfural derivatives and sugar alcohols by using heterogeneous catalysts.

    Science.gov (United States)

    Dabral, Saumya; Nishimura, Shun; Ebitani, Kohki

    2014-01-01

    Inedible and/or waste biomass reserves are being strongly focused upon as a suitable new energy and chemical source. Raffinose, which is an indigestible trisaccharide composed of glucose, galactose, and fructose, is found abundantly in beet molasses, sugar cane, and seeds of many leguminous plants. Herein, we demonstrate the one-pot synthesis of furan derivatives and sugar alcohols from raffinose by using heterogeneous acid, base, and/or metal-supported catalysts. The combination of Amberlyst-15 and hydrotalcite (HT) showed a high activity (37% yield) for 5-hydroxymethyl-2-furaldehyde (HMF) through continuous hydrolysis, isomerization, and dehydration reactions. In addition, the use of a hydrotalcite-supported ruthenium catalyst (Ru/HT) successfully afforded 2,5-diformylfuran (DFF, 27% yield) from HMF produced by raffinose, directly. Moreover, the hydrogenation of hexoses obtained by raffinose hydrolysis into sugar alcohols (galactitol, mannitol, sorbitol) was also achieved in a high yield (91%) with Amberlyst-15 and Ru/HT catalysts. Thus, we suggest that raffinose has great potential for the synthesis of important industrial intermediates under mild reaction conditions. PMID:24193816

  9. 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. PMID:27561496

  10. One-pot synthesis of magnetic nanoclusters enabling atherosclerosis-targeted magnetic resonance imaging

    Directory of Open Access Journals (Sweden)

    Kukreja A

    2014-05-01

    Full Text Available Aastha Kukreja,1 Eun-Kyung Lim,2–4 Byunghoon Kang,1 Yuna Choi,2 Taeksu Lee,1 Jin-Suck Suh,2,3 Yong-Min Huh,2,3 Seungjoo Haam1,31Department of Chemical and Biomolecular Engineering, College of Engineering, 2Department of Radiology, College of Medicine, Yonsei University, Seoul, Republic of Korea; 3YUHS-KRIBB Medical Convergence Research Institute, Seoul, Republic of Korea; 4BioNanotechnology Research Center, Korea Research Institute of Bioscience and Biotechnology, Daejeon, Republic of KoreaAbstract: In this study, dextran-encrusted magnetic nanoclusters (DMNCs were synthesized using a one-pot solution phase method for detection of atherosclerosis by magnetic resonance imaging. Pyrenyl dextran was used as a surfactant because of its electron-stabilizing effect and its amphiphilic nature, rendering the DMNCs stable and water-dispersible. The DMNCs were 65.6±4.3 nm, had a narrow size distribution, and were superparamagnetic with a high magnetization value of 60.1 emu/g. Further, they showed biocompatibility and high cellular uptake efficiency, as indicated by a strong interaction between dextran and macrophages. In vivo magnetic resonance imaging demonstrated the ability of DMNCs to act as an efficient magnetic resonance imaging contrast agent capable of targeted detection of atherosclerosis. In view of these findings, it is concluded that DMNCs can be used as magnetic resonance imaging contrast agents to detect inflammatory disease.Keywords: magnetic nanocrystal, magnetic resonance imaging, atherosclerosis, macrophages, dextran

  11. One-pot conversions of raffinose into furfural derivatives and sugar alcohols by using heterogeneous catalysts.

    Science.gov (United States)

    Dabral, Saumya; Nishimura, Shun; Ebitani, Kohki

    2014-01-01

    Inedible and/or waste biomass reserves are being strongly focused upon as a suitable new energy and chemical source. Raffinose, which is an indigestible trisaccharide composed of glucose, galactose, and fructose, is found abundantly in beet molasses, sugar cane, and seeds of many leguminous plants. Herein, we demonstrate the one-pot synthesis of furan derivatives and sugar alcohols from raffinose by using heterogeneous acid, base, and/or metal-supported catalysts. The combination of Amberlyst-15 and hydrotalcite (HT) showed a high activity (37% yield) for 5-hydroxymethyl-2-furaldehyde (HMF) through continuous hydrolysis, isomerization, and dehydration reactions. In addition, the use of a hydrotalcite-supported ruthenium catalyst (Ru/HT) successfully afforded 2,5-diformylfuran (DFF, 27% yield) from HMF produced by raffinose, directly. Moreover, the hydrogenation of hexoses obtained by raffinose hydrolysis into sugar alcohols (galactitol, mannitol, sorbitol) was also achieved in a high yield (91%) with Amberlyst-15 and Ru/HT catalysts. Thus, we suggest that raffinose has great potential for the synthesis of important industrial intermediates under mild reaction conditions.

  12. Microwave-assisted one-pot synthesis of 1,6-anhydrosugars and orthogonally protected thioglycosides.

    Science.gov (United States)

    Ko, Yen-Chun; Tsai, Cheng-Fang; Wang, Cheng-Chung; Dhurandhare, Vijay M; Hu, Pu-Ling; Su, Ting-Yang; Lico, Larry S; Zulueta, Medel Manuel L; Hung, Shang-Cheng

    2014-10-15

    Living organisms employ glycans as recognition elements because of their large structural information density. Well-defined sugar structures are needed to fully understand and take advantage of glycan functions, but sufficient quantities of these compounds cannot be readily obtained from natural sources and have to be synthesized. Among the bottlenecks in the chemical synthesis of complex glycans is the preparation of suitably protected monosaccharide building blocks. Thus, easy, rapid, and efficient methods for building-block acquisition are desirable. Herein, we describe routes directly starting from the free sugars toward notable monosaccharide derivatives through microwave-assisted one-pot synthesis. The procedure followed the in situ generation of per-O-trimethylsilylated monosaccharide intermediates, which provided 1,6-anhydrosugars or thioglycosides upon treatment with either trimethylsilyl trifluoromethanesulfonate or trimethyl(4-methylphenylthio)silane and ZnI2, respectively, under microwave irradiation. We successfully extended the methodology to regioselective protecting group installation and manipulation toward a number of thioglucosides and the glycosylation of persilylated derivatives, all of which were conducted in a single vessel. These developed approaches open the possibility for generating arrays of suitably protected building blocks for oligosaccharide assembly in a short period with minimal number of purification stages. PMID:25291402

  13. 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.

  14. Symmetry breaking polymerization: one-pot synthesis of plasmonic hybrid Janus nanoparticles.

    Science.gov (United States)

    Wang, Yanming; Ding, Tao; Baumberg, Jeremy J; Smoukov, Stoyan K

    2015-06-21

    Asymmetric hybrid nanoparticles have many important applications in catalysis, nanomotion, sensing, and diagnosis, however ways to generate the asymmetric hybrid nanoparticles are quite limited and inefficient. Most current methods rely on interfacial adhesion and modification of already formed particles. In this article we report a one-pot, facile and scalable synthesis of anisotropic Au-polymer hybrid nanoparticles via interfacial oxidative dispersion polymerization. The interfacial nucleation and polymerization lead to spontaneous symmetry breaking and formation of the Janus particles. The reaction is initiated by monomer radicals generated by the strong oxidant HAuCl4, which is itself later reduced by the electron-rich monomers to self-nucleate and form Au nanoparticles (NPs). The competition between divinylbenzene adsorption and the PVP capping agent results in effective partial surface wetting, forming asymmetric Au-PDVB hybrid nanoparticles, by confining growth of each material to its own phase. Such spontaneous symmetry breaking, important in morphogenesis, with control over the subsequent growth processes should lead to significant advances in the synthesis of asymmetric nanostructures.

  15. One-pot synthesis of reduced graphene oxide-cadmium sulfide nanocomposite and its photocatalytic hydrogen production.

    Science.gov (United States)

    Zeng, Peng; Zhang, Qinggang; Peng, Tianyou; Zhang, Xiaohu

    2011-12-28

    Reduced graphene oxide (RGO)-cadmium sulfide (CdS) nanocomposites were successfully prepared by a one-pot solvothermal process without pretreatment of graphene oxide (GO) and a precipitation process, in which GO needs to be pre-reduced by hydrazine. The as-obtained RGO-CdS nanocomposites were used as photocatalysts for hydrogen production under visible light irradiation, and it was found that the product derived from the one-pot solvothermal process showed much better photoactivity than that from the precipitation method. PMID:22068902

  16. One-pot synthesis of S-alkyl dithiocarbamates via the reaction of N-tosylhydrazones, carbon disulfide and amines.

    Science.gov (United States)

    Sha, Qiang; Wei, Yun-Yang

    2013-09-14

    A new, convenient and efficient transition metal-free synthesis of S-alkyl dithiocarbamates through one-pot reaction of N-tosylhydrazones, carbon disulfide and amines is reported. Tosylhydrazones derived from various aromatic and aliphatic ketones or aldehydes were tested and gave dithiocarbamates in good to excellent yields. The tosylhydrazones can be generated in situ without isolation, which provides a simpler one-pot method to synthesize dithiocarbamates via the reaction of carbonyl compounds, carbon disulfide and amines in the presence of 4-methylbenzenesulfonohydrazide. PMID:23863979

  17. One-pot multi-component synthesis of 1,4-dihydropyridine derivatives in biocompatible deep eutectic solvents

    Indian Academy of Sciences (India)

    Suhas Pednekar; Rahul Bhalerao; Nitin Ghadge

    2013-05-01

    An efficient protocol for the synthesis of differently substituted 1, 4-dihydropyridines in deep eutectic solvents under solvent-free conditions is reported here. Excellent yields of the resultant products have been obtained. Recyclability studies have also been performed for deep eutectic solvents with very little loss in activity up to five recycles.

  18. Nonionic metal-chelating surfactants mediated solvent-free thermo-induced separation of uranyl

    Energy Technology Data Exchange (ETDEWEB)

    Larpent, Ch.; Prevost, S. [Versailles-St-Quentin Univ., Institut Lavoisier, UMR-CNRS 8180, 78 - Versailles (France); Prevost, S.; Zemb, Th.; Testard, F. [CEA Saclay, Dept. de Recherche sur l' Etat Condense, les Atomes et les Molecules (DSM/DRECAM/SCM/LIONS), 91 - Gif sur Yvette (France); Berthon, L. [CEA Valrho, Site de Marcoule, Dept. Radiochimie et Procedes (DEN/DRCP/SCPS/LCSE), 30 (France)

    2007-08-15

    Thermo-responsive metal-chelating surfactants permit the solvent-free, cloud point extraction of uranyl nitrate and afford a real molecular economy compared to conventional separation techniques. (authors)

  19. One pot synthesis of N-ethylaniline from nitrobenzene and ethanol

    Institute of Scientific and Technical Information of China (English)

    LI XiaoNian; ZHANG JunHua; XIANG YiZhi; MA Lei; ZHANG QunFeng; LU ChunShan; WANG Hong; BAI Ying

    2008-01-01

    A novel method for the one pot synthesis of N-alkyl arylamines from nitro aromatic compounds and alcohols is proposed through the combination of the aqueous-phase reforming of alcohol for hydrogen production, the reduction of nitro aromatic compounds for the synthesis of aromatic amine and the N-alkylation of aromatic amine for the production of N-alkyl arylamine over an identical catalyst under the same conditions of temperature and pressure in a single reactor. In this process, hydrogen gener-ated from the aqueous-phase reforming of alcohols was used in-situ for the hydrogenation of nitro aromatic compounds for aromatic amine synthesis, followed by N-alkylation of aromatic amine with alcohols to form the corresponding N-alkyl arylamines at a low partial pressure of hydrogen. For the system composed of nitrobenzene and ethanol, under the conditions of 413 K and PN2=1 MPa, the conversion degrees of nitrobenzene and aniline were 100%, the selectivity to N-ethylaniline and N, N-diethylaniline were 85.9% and 0%-4%, respectivity, after reaction for 8 h at the volumetric ratio of nitrobenzene: ethanol :water = 10:60: 0. The selectivity for N, N-diethylaniline production is much lower than that through the traditional method. In this process, hydrogen and aromatic amines generated from the aqueous-phase reforming of alcohols and hydrogenation of nitro aromatic compounds, re-spectively, could be promptly removed from the surface of the catalyst due to the occurrence of in-situ hydrogenation and N-alkylation reactions. Thus, this may be a potential approach to increase the se-lectivity to N-alkyl arylamine.

  20. One pot synthesis of N-ethylaniline from nitrobenzene and ethanol

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A novel method for the one pot synthesis of N-alkyl arylamines from nitro aromatic compounds and alcohols is proposed through the combination of the aqueous-phase reforming of alcohol for hydrogen production, the reduction of nitro aromatic compounds for the synthesis of aromatic amine and the N-alkylation of aromatic amine for the production of N-alkyl arylamine over an identical catalyst under the same conditions of temperature and pressure in a single reactor. In this process, hydrogen generated from the aqueous-phase reforming of alcohols was used in-situ for the hydrogenation of nitro aromatic compounds for aromatic amine synthesis, followed by N-alkylation of aromatic amine with alcohols to form the corresponding N-alkyl arylamines at a low partial pressure of hydrogen. For the system composed of nitrobenzene and ethanol, under the conditions of 413 K and PN2 = 1 MPa, the conversion degrees of nitrobenzene and aniline were 100%, the selectivity to N-ethylaniline and N, N-diethylaniline were 85.9% and 0%-4%, respectivity, after reaction for 8 h at the volumetric ratio of nitrobenzene:ethanol:water = 10:60:0. The selectivity for N, N-diethylaniline production is much lower than that through the traditional method. In this process, hydrogen and aromatic amines generated from the aqueous-phase reforming of alcohols and hydrogenation of nitro aromatic compounds, respectively, could be promptly removed from the surface of the catalyst due to the occurrence of in-situ hydrogenation and N-alkylation reactions. Thus, this may be a potential approach to increase the selectivity to N-alkyl arylamine.

  1. One-pot preparation of Ni-graphene hybrids with enhanced catalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Guiqiang, E-mail: chengphnu@126.com [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China); Wang, Fengli [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China); Liu, Fei [Department of Electrical Engineering, Zhangjiakou Vocational College of Technology, Zhangjiakou 075000, Hebei (China); Zhang, Xiao, E-mail: Zhangxiao83690@163.com [College of Information Science and Engineering, Hebei North University, Zhangjiakou 075000, Hebei (China)

    2014-10-15

    Highlights: • Ni-rGO hybrids were synthesized by a microwave-assisted method. • NaBH4 was used as a reducing agent to fabricate Ni-rGO hybrids. • Ni-rGO was used as catalyst for the reduction of p-nitrophenol. • Ni-rGO showed higher catalytic ability than pure Ni nanoparticles. • Ni-rGO showed good recyclability and stability. - Abstract: A facile one-pot method was developed to synthesize magnetic nickel nanoparticles (Ni NPs) decorated on reduced graphene oxide (rGO) with NaHB{sub 4} as a reductant under microwave irradiation. The morphologies and structures of the Ni-rGO hybrids were investigated by electron microscopy, thermal gravimetric analysis, X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectroscopy and magnetic measurements. The results showed that Ni-rGO hybrids composed of the well-dispersed Ni NPs with an average diameter of 12 nm were successfully prepared. To demonstrate one potential application, the catalytic ability of Ni-rGO was evaluated and it was found that Ni-rGO showed much enhanced catalytic ability, good recyclability and stability toward the catalytic reduction of p-nitrophenol to p-aminophenol. The excellent catalytic activity of Ni-rGO hybrids was due possibly to the synergistic effect of Ni NPs and rGO, including the uniform distribution of Ni NPs onto rGO, enhanced electrons separation and transport, as well as the fast adsorption of p-nitrophenol by rGO.

  2. 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.

  3. Zinc chloride catalyzed synthesis of 5-substituted 1H-tetrazoles under solvent free condition

    Institute of Scientific and Technical Information of China (English)

    Shahnaz Rostamizadeh; Hamid Ghaieni; Reza Aryan; Ali Amani

    2009-01-01

    Zinc chloride is an efficient and safe catalyst in the [3 + 2] cycloaddition reaction of organic nitriles with sodium azide in solventless condition. The corresponding 5-substituted IH tetrazoles were obtained under mild conditions. This method can overcome disadvantages such as: the use of toxic metals and expensive reagents, drastic reaction conditions, water sensitivity and the presence of dangerous hydrazoic acid.

  4. Sulfanilic acid catalyzed solvent-free synthesis of 1,5-benzodiazepine derivatives

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Sulfanilic acid has been found to be an efficient catalyst for the synthesis of 1,5-benzodiazepines from o-phenylenediamine and ketones. This method is simple, effective and environmentally friendly and gives better yields.

  5. A Novel Synthesis of Biscoumarin Derivatives Catalyzed by Zncl2 Under Solvent-Free Conditions

    OpenAIRE

    Vahid Vahabi; Farhad Hatamjafari

    2014-01-01

    Zinc chloride (ZnCl2) is used as an efficient catalyst condensation of 4-hydroxycoumarin and with various aromatic aldehydes leading to the formation of biscoumarin derivatives. Easy isolation of the products, short reaction times, excellent yields and reusability of catalyst was theadvantage of thismethod.

  6. 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....

  7. A facile one-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica: Aqueous hydration of nitriles to amides

    Science.gov (United States)

    One-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica is described which involve the in situ generation of magnetic silica (Fe3O4@ SiO2) and ruthenium hydroxide immobilization; the hydration of nitriles occurs in high yield and excellent selectivity using this...

  8. A facile one pot strategy for the synthesis of well-defined polyacrylates from acrylic acid via RAFT polymerization.

    Science.gov (United States)

    Li, Qianbiao; Wang, Taisheng; Dai, Jingwen; Ma, Chao; Jin, Bangkun; Bai, Ruke

    2014-03-28

    A facile one pot strategy for the preparation of linear and hyperbranched polyacrylates has been successfully developed by the combination of in situ esterification of acrylic acid with halogenated compounds promoted by 1,1,3,3-tetramethylguanidine (TMG) and RAFT polymerization. PMID:24534953

  9. One-pot synthesis of N-aryl 1,4-dihydropyridine derivatives and their biological activities

    Indian Academy of Sciences (India)

    Isaivani Dhinakaran; Vediappen Padmini; Nattamai Bhuvanesh

    2015-12-01

    Highly efficient, one pot synthesis of N-aryl, 1,4-dihydopyridines was carried out by four component reaction. Synthesized 1,4-dihydropyridines were screened for their cytotoxicity against A549 cell line. All the synthesized compounds exhibited better DPPH radical scavenging activity.

  10. Efficient one-pot synthesis of 2-oxazolines from benzoylacetonitrile and -aminoalcohols mediated by ZnCl2

    Indian Academy of Sciences (India)

    Mei Luo; Jing Cheng Zhang; Hao Yin

    2015-01-01

    A series of 2-oxazolines were synthesized using a simple, one-pot method under inert, moisturefree conditions from the benzoylacetonitrile and -aminoalcohols mediated by 115-172 mol% ZnCl2. Structures of products were fully characterized by NMR, IR and MS.

  11. Silver iodide nanoparticle as an efficient and reusable catalyst for the one-pot synthesis of benzofurans under aqueous conditions

    Indian Academy of Sciences (India)

    Javad Safaei-Ghomi; Mohammad Ali Ghasemzadeh

    2013-09-01

    Recyclable heterogeneous AgI nanoparticles were efficiently catalysed one-pot three-component reaction of aldehydes, secondary amines and alkyne in aqueous media. This method provides a novel and improved approach for the synthesis of 2,3-disubstituted benzo[b]furan derivatives to obtain excellent yields, short reaction times and low catalyst loading.

  12. Metal-free one-pot synthesis of 2-substituted and 2,3-disubstituted morpholines from aziridines

    Directory of Open Access Journals (Sweden)

    Hongnan Sun

    2015-04-01

    Full Text Available The metal-free synthesis of 2-substituted and 2,3-disubstituted morpholines through a one-pot strategy is described. A simple and inexpensive ammonium persulfate salt enables the reaction of aziridines with halogenated alcohols to proceed via an SN2-type ring opening followed by cyclization of the resulting haloalkoxy amine.

  13. Metal-free one-pot synthesis of 2-substituted and 2,3-disubstituted morpholines from aziridines

    OpenAIRE

    Hongnan Sun; Binbin Huang; Run Lin; Chao Yang; Wujiong Xia

    2015-01-01

    The metal-free synthesis of 2-substituted and 2,3-disubstituted morpholines through a one-pot strategy is described. A simple and inexpensive ammonium persulfate salt enables the reaction of aziridines with halogenated alcohols to proceed via an SN2-type ring opening followed by cyclization of the resulting haloalkoxy amine.

  14. Facile one-pot synthesis of multi-yolk-shell Bi@C nanostructures by the nanoscale Kirkendall effect.

    Science.gov (United States)

    Cui, C M; Guo, X H; Geng, Y M; Dang, T T; Xie, G; Chen, S P; Zhao, F Q

    2015-06-01

    Multi-yolk-shell Bi@C nanostructures were prepared via a facile one-pot template-free hydrothermal approach. The prepared Bi@C nanostructures can act as a solid catalyst in the thermal decomposition of cyclotrimethylenetrinitramine (RDX) and display excellent catalytic activity, which highlights their application in the field of energetic materials.

  15. ZnO Nanoparticles: An Efficient Reagent, Simple and One-Pot Procedure for Synthesis of Highly Functionalized Dihydropyridine Derivatives

    OpenAIRE

    Khazaei, Marziyeh; Anary-Abbasinejad, Mohammad; Hassanabadi, Alireza; Sadeghi, Bahareh

    2012-01-01

    A new and efficient one-pot synthesis of dihydropyridones derivatives by four-component reaction between cyanoacetamide, aryl aldehydes, and ethyl acetoacetate with ammonium acetate using nano ZnO is described. The reaction was performed in ethanol under reflux conditions and afforded good yields of products.

  16. One-pot synthesis of quinaldine derivatives by using microwave irradiation without any solvent - A green chemistry approach

    Indian Academy of Sciences (India)

    Javad Safari; Sayed Hossein Banitaba; Sepehr Sadegh Samiei

    2009-07-01

    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.

  17. One-pot synthesis of novel 1, 8-dioxo-decahydroacridines containing phenol and benzamide moiety and their synthetic uses

    Indian Academy of Sciences (India)

    Ali Dorehgiraee; Esmat Tavakolinejad Kermani; Hojatollah Khabazzadeh

    2014-07-01

    An efficient synthesis of some new 1, 8-dioxo-decahydroacridines is achieved via one-pot, threecomponent condensation of aromatic aldehydes, cyclic diketone, and 4-amino benzamide/4-aminophenol. Reaction of these acridines with dimethylacetylene dicarboxylate and triphenylphosphine or cyclohexylisocyanide gives stable phosphorus ylides or 4H-chromene derivatives, respectively, with good yields.

  18. Synthesis and anti-inflammatory activity of 3-indolyl pyridine derivatives through one-pot multi component reaction

    Indian Academy of Sciences (India)

    Prakasam Thirumurugan; S Mahalaxmi; Paramasivan T Perumal

    2010-11-01

    A simple protocol for the efficient preparation of 2-(1-Indol-3-yl)-6-methoxy-4-arylpyridine-3,5-dicarbonitrile has been achieved through one-pot multi-component reaction under reflux condition. These compounds showed a good anti-inflammatory activity. Also a series of bis-Hantzsch dihydropyridine derivatives were synthesized and they exhibit analgesic activity.

  19. 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...

  20. One-pot bioethanol production from cellulose by co-culture of Acremonium cellulolyticus and Saccharomyces cerevisiae

    Directory of Open Access Journals (Sweden)

    Park Enoch Y

    2012-08-01

    Full Text Available Abstract Background While the ethanol production from biomass by consolidated bioprocess (CBP is considered to be the most ideal process, simultaneous saccharification and fermentation (SSF is the most appropriate strategy in practice. In this study, one-pot bioethanol production, including cellulase production, saccharification of cellulose, and ethanol production, was investigated for the conversion of biomass to biofuel by co-culture of two different microorganisms such as a hyper cellulase producer, Acremonium cellulolyticus C-1 and an ethanol producer Saccharomyces cerevisiae. Furthermore, the operational conditions of the one-pot process were evaluated for maximizing ethanol concentration from cellulose in a single reactor. Results Ethanol production from cellulose was carried out in one-pot bioethanol production process. A. cellulolyticus C-1 and S. cerevisiae were co-cultured in a single reactor. Cellulase producing-medium supplemented with 2.5 g/l of yeast extract was used for productions of both cellulase and ethanol. Cellulase production was achieved by A. cellulolyticus C-1 using Solka-Floc (SF as a cellulase-inducing substrate. Subsequently, ethanol was produced with addition of both 10%(v/v of S. cerevisiae inoculum and SF at the culture time of 60 h. Dissolved oxygen levels were adjusted at higher than 20% during cellulase producing phase and at lower than 10% during ethanol producing phase. Cellulase activity remained 8–12 FPU/ml throughout the one-pot process. When 50–300 g SF/l was used in 500 ml Erlenmeyer flask scale, the ethanol concentration and yield based on initial SF were as 8.7–46.3 g/l and 0.15–0.18 (g ethanol/g SF, respectively. In 3-l fermentor with 50–300 g SF/l, the ethanol concentration and yield were 9.5–35.1 g/l with their yields of 0.12–0.19 (g/g respectively, demonstrating that the one-pot bioethanol production is a reproducible process in a scale-up bioconversion of cellulose to ethanol

  1. 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.

  2. A novel polymeric catalyst for the one-pot synthesis of 2,4,5-triaryl-1H-imidazoles

    Indian Academy of Sciences (India)

    Ali Mohammadi; Hossein Keshvari; Reza Sandaroos; Hamed Rouhi; Zeinalabedin Sepehr

    2012-05-01

    An efficient synthesis of 2,4,5-trisubstituted imidazoles is achieved by three component cyclocondensation 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 reaction times, easy work-up, purification of products by non-chromatographic method and the reusability of the catalyst.

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

    Science.gov (United States)

    Silveira-Dorta, Gastón; Álvarez-Méndez, Sergio J; Martín, Víctor S

    2016-01-01

    Summary 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-(dia)stereoselectivity was observed when compared to the previous one-pot method. The (dia)stereoselectivity 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. PMID:27340486

  4. Controlled synthesis of multi-shelled transition metal oxide hollow structures through one-pot solution route

    Institute of Scientific and Technical Information of China (English)

    Xi Wang; Yi-Jun Yang; Ying Ma; Jian-Nian Yao

    2013-01-01

    As one type of promising candidates fot environmental and energy-related systems,multi-shelled transition metal oxide hollow structures (MS-TMOHSs) have drawn great scientific and technical interest in the past few years.This article highlights recent advances in one-pot solution synthesis of MS-TMOHSs.We begin it with an overview of synthetic strategies that have been exploited to achieve these peculiar structures.We then focus on one-pot solution approaches in the following four sections:i) soft templates directed growth; ii) Ostwald ripening; iii) controlled etching; and iv) gas bubble assisted growth.After giving a brief discussion on the unique properties and applications of these multi-shelled hollow structures,we conclude this review with the general challenges and the potential future directions of this exciting area of research.

  5. One-pot five-component synthesis of highly functionalized piperidines using oxalic acid dihydrate as a homogenous catalyst

    Institute of Scientific and Technical Information of China (English)

    Seyed Sajad Sajadikhah; Malek Taher Maghsoodlou; Nourallah Hazeri; Sayyed Mostafa Habibi-Khorassani; Anthony C. Willis

    2012-01-01

    An efficient green protocol is described for the preparation of highly functionalized piperidines via a one-pot five-component reaction between aromatic aldehydes,anilines and β-ketoesters in the presence of oxalic acid dihydrate as catalyst in ethanol at ambient temperature.The structure as well as the relative stereochemistry of these compounds was confirmed by single X-ray crystallographic analysis.

  6. One-pot three-component synthesis of quinoxaline and phenazine ring systems using Fischer carbene complexes

    Directory of Open Access Journals (Sweden)

    Priyabrata Roy

    2010-05-01

    Full Text Available One-pot three-component coupling of o-alkynylheteroaryl carbonyl derivatives with Fischer carbene complexes and dienophiles leading to the synthesis of quinoxaline and phenazine ring systems has been investigated. This involves the generation of furo[3,4-b]pyrazine and furo[3,4-b]quinoxaline as transient intermediates, which were trapped with Diels–Alder dienophiles. This is the first report on furo[3,4-b]pyrazine intermediates.

  7. A new one-pot synthesis of 1,2,4-oxadiazoles from aryl nitriles, hydroxylamine and crotonoyl chloride

    Indian Academy of Sciences (India)

    Masoumeh Zakeri; Majid M Heravi; Ebrahim Abouzari-Lotf

    2013-07-01

    The reaction of aryl nitriles with hydroxylamine using acetic acid as a catalyst followed by subsequent addition of crotonoyl chloride to the intermediate amidoxime represents a straightforward one-pot access to new 1,2,4-oxadiazole synthesis under mild conditions. The course of the reaction was found to be high yielding and all new compounds were well characterized by nuclear magnetic resonance (NMR), mass spectrometry (MS) and elemental analysis.

  8. A Simple One-pot Synthesis of 3,5-Dicyano-1,2-dihydropyrid-2-ones in Aqueous Media

    Institute of Scientific and Technical Information of China (English)

    ZHUANG, Qi-Ya; XU, Jia-Ning; TU, Shu-Jiang; JIA, Run-Hong; ZHANG, Jun-Yong; LI, Chun-Mei; ZHOU, Dian-Xiang

    2007-01-01

    A simple and clean synthesis of 3,5-dicyano-1,2-dihydropyrid-2-ones by a one-pot three-component reaction of malononitrile, aromatic aldehydes and 2-cyanoacetamide or 2-cyanothioacetamide has been achieved in an aqueous solution with potassium carbonate as a base under microwave irradiation without a phase transfer reagent. This protocol has the advantages of short reaction time (5-8 min) and convenient work-up.

  9. One-Pot Synthesis, Encaspulation, and Solubilization of Size-Tuned Quantum Dots with Amphiphilic Multidentate Ligands

    OpenAIRE

    Kairdolf, Brad A.; SMITH, ANDREW M.; Nie, Shuming

    2008-01-01

    We report one-pot synthesis, encapsulation, and solubilization of high-quality quantum dots based on the use of amphiphilic and multidentate polymer ligands. In this “all-in-one” procedure, the resulting QDs are first capped by the multidentate ligand, and are then spontaneously encapsulated and solubilized by a second layer of the same multidentate polymer upon exposure to water. In addition to providing better control of nanocrystal nucleation and growth kinetics (including resistance to Os...

  10. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    OpenAIRE

    Ezzaldeen Younes Jomma; Shou-Nian Ding

    2016-01-01

    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 resultan...

  11. One-pot synthesis of molecular bottle-brush functionalized single-walled carbon nanotubes with superior dispersibility in water.

    Science.gov (United States)

    Deng, Yong; Hu, Qin; Yuan, Qiulin; Wu, Yan; Ling, Ying; Tang, Haoyu

    2014-01-01

    Molecular bottle-brush functionalized single-walled carbon nanotubes (SWCNTs) with superior dispersibility in water are prepared by a one-pot synthetic methodology. Elongating the main-chain and side-chain length of molecular bottle-brushes can further increase SWCNT dispersibility. They show significant enhancement of SWCNT dispersibility up to four times higher than those of linear molecular functionalized SWCNTs. PMID:24307218

  12. Reduced Species(HSO-2,SO·-2)Promoted One-Pot Efficient Synthesis of Phenyl Alkyl Selenides

    Institute of Scientific and Technical Information of China (English)

    TANG,Ri-Yuan; ZHONG,Ping; LIN,Qiu-Lian

    2007-01-01

    Reduced species(HSO-2,SO·-2)promoted one-pot synthesis of phenyl alkyl selenides has been developed.This synthetic method was achieved by reactions of diphenyl diselenide with alkyl halides at room temperature.It is noteworthy that the reactions were operated under mild reaction conditions,required short time,and got good resuits.A single electron transfer reaction mechanism was proposed for the reaction.

  13. One-pot hydrothermal synthesis of zeolite/sodium tantalate composite and its photodegradation of methyl orange

    Energy Technology Data Exchange (ETDEWEB)

    Gu, Xiaoli [College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037 (China); Key Laboratory of Energy Thermal Conversion and Control of Ministry of Education, Southeast University, Nanjing 210096 (China); Lu, Haiqiang [School of Chemical and Biological Engineering, Taiyuan University of Science and Technology, Taiyuan 030021 (China); Kan, Chun [College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037 (China); Yao, Jianfeng, E-mail: jfyao@njfu.edu.cn [College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037 (China); Department of Chemical Engineering, Monash University, Clayton, VIC 3800 (Australia)

    2015-08-15

    Highlights: • Sodalite/NaTaO{sub 3} composite is prepared by a one-pot hydrothermal synthesis. • Enhanced photodegradation is achieved due to the heterogeneous doping effect. • Structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing. - Abstract: Sodalite/NaTaO{sub 3} composite was prepared by a one-pot hydrothermal synthesis method. Sodalite and NaTaO{sub 3} grow interpenetrated, and the resulting composites have similar morphology as the pure sodalite. The sodalite/NaTaO{sub 3} composite has a lower band gap of 3.35 eV due to the heterogeneous doping effect, and exhibits an enhanced photodegradation of methyl orange under UV irradiation as compared to the pure NaTaO{sub 3}. A slight structure distortion is found for NaTaO{sub 3} after removing sodalite by acid washing the sodalite/NaTaO{sub 3} composite, and such result further confirms the co-growth of the two crystals. This one-pot hydrothermal method opens up new avenues for the preparation of photocatalytic composites.

  14. A novel inorganic-organic nanohybrid material H4SiW12O40/pyridino-MCM-41 as efficient catalyst for the preparation of 1-amidoalkyl-2-naphthols under solvent-free conditions.

    Science.gov (United States)

    Tayebee, R; Amini, M M; Akbari, M; Aliakbari, A

    2015-05-28

    A new inorganic-organic nanohybrid material H4SiW12O40/pyridino-MCM-41 was prepared and performed as an efficient, eco-friendly, and highly recyclable catalyst for the one-pot multi-component synthesis of different substituted 1-amidoalkyl-2-naphthols under solvent-free conditions. The nanohybrid catalyst was prepared through electrostatic anchoring of Keggin heteropolyacid H4SiW12O40 on the surface of MCM-41 nanoparticles modified by N-[3-(triethoxysilyl)propyl]isonicotinamide. The prepared material was characterized by XRD, SEM, EDX, UV-Vis, DTA-TGA, DLS, and FT-IR spectroscopy. Findings confirmed that the heteropolyacid is well dispersed on the surface of the solid support and its structure is preserved after immobilization on the TPI modified MCM-41 nanoparticles. The recovered catalyst was easily recycled for at least seven runs without considerable loss of catalytic activity. PMID:25923593

  15. 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.

  16. One-Pot Synthesis of (S)-Baclofen via Aldol Condensation of Acetaldehyde with Diphenylprolinol Silyl Ether Mediated Asymmetric Michael Reaction as a Key Step.

    Science.gov (United States)

    Hayashi, Yujiro; Sakamoto, Daisuke; Okamura, Daichi

    2016-01-01

    An efficient asymmetric total synthesis of (S)-baclofen was accomplished via a one-pot operation from commercially available materials using sequential reactions, such as aldol condensation of acetaldehyde, diphenylprolinol silyl ether mediated asymmetric Michael reaction of nitromethane, Kraus-Pinnick oxidation, and Raney Ni reduction. Highly enantioenriched baclofen was obtained in one pot with a good yield over four reactions. PMID:26636719

  17. One-pot solvothermal synthesis of a well-ordered layered sodium aluminoalcoholate complex: a useful precursor for the preparation of porous Al2O3 particles

    Energy Technology Data Exchange (ETDEWEB)

    Li, XS; Michaelis, VK; Ong, TC; Smith, SJ; McKay, I; Muller, P; Griffin, RG; Wang, EN

    2014-01-01

    One-pot solvothermal synthesis of a robust tetranuclear sodium hexakis(glycolato)tris(methanolato)aluminate complex Na-3[Al-4(OCH3)(3)(OCH2CH2O)(6)] via a modified yet rigorous base-catalyzed transesterification mechanism is presented here. Single crystal X-ray diffraction (SCXRD) studies indicate that this unique Al complex contains three pentacoordinate Al3+ ions, each bound to two bidentate ethylene glycolate chelators and one monodentate methanolate ligand. The remaining fourth Al3+ ion is octahedrally coordinated to one oxygen atom from each of the six surrounding glycolate chelators, effectively stitching the three pentacoordinate Al moieties together into a novel tetranuclear Al complex. This aluminate complex is periodically self-assembled into well-ordered layers normal to the [110] axis with the intra-/inter-layer bonding involving extensive ionic bonds from the three charge-counterbalancing Na+ cations rather than the more typical hydrogen bonding interactions as a result of fewer free hydroxyl groups present in its structure. It can also serve as a valuable precursor toward the facile synthesis of high-surface-area alumina powders using a very efficient rapid pyrolysis technique.

  18. Fabrication of stable photovoltachromic cells using a solvent-free hybrid polymer electrolyte.

    Science.gov (United States)

    Yang, Ming-Che; Cho, Hsun-Wei; Wu, Jih-Jen

    2014-08-21

    In this work, photovoltachromic cells (PVCCs) are fabricated using a solvent-free polyethylene glycol (PEG)-titanium hybrid polymer electrolyte. With appropriate addition of 1,2-dimethyl-3-propylimidazolium iodide in the electrolyte, the range of tunable colored-state transmittance of the PVCC is enlarged due to an improved fill factor. A transmittance modulation larger than 40% can be maintained for at least 3 months, demonstrating the good long-term stability of PVCCs fabricated using the solvent-free PEG-Ti hybrid electrolyte.

  19. Three-component synthesis of amidoalkyl naphthols catalyzed by bismuth(Ⅲ) nitrate pentahydrate

    Institute of Scientific and Technical Information of China (English)

    Min Wang; Yan Liang; Ting Ting Zhang; Jing Jing Gao

    2012-01-01

    Bismuth(Ⅲ) nitrate pentahydrate catalyzed the three-component condensation of β-naphthol,aldehydes and amines/urea under solvent-free conditions to afford the corresponding amidoalkyl naphthols in excellent yields.

  20. Microwave-assisted silica-promoted solvent-free synthesis of triazoloquinazolinone and benzimidazoquinazolinones

    Indian Academy of Sciences (India)

    G Krishnamurthy; K V Jagannath

    2013-07-01

    The derivative of triazolo/benzimidazoquinazolinones is prepared via silica-promoted solvent-free method using microwave irradiation with an excellent yield. The newly synthesized compounds were characterized by various techniques like IR, NMR and Mass spectroscopy. The compound with 1a was crystallized and analysed by single crystal X-ray diffraction studies.

  1. Solvent-free microwave extraction of bioactive compounds provides a tool for green analytical chemistry

    OpenAIRE

    Ying LI; Fabiano-Tixier, Anne-Sylvie; Vian, Maryline; Chemat, Farid

    2013-01-01

    We present an overview on solvent-free microwave-extraction techniques of bioactive compounds from natural products. This new technique is based on the concept of green analytical chemistry. It has proved to be an alternative to other techniques with the advantages of reducing extraction times, energy consumption, solvent use and CO2 emissions.

  2. 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.

  3. Solvent-free Reactions of Formylferrocene with Active Methylene Containing Compounds

    Institute of Scientific and Technical Information of China (English)

    BAI Yin-Juan; GAN Hai-Ying; LU Jun; SHI Zhen

    2003-01-01

    @@ Since ferrocene was synthesized, derivatives of ferrocene have attracted the attention of chemists, and recently solvent-free organic reaction has been an important new dimension in preparative organic chemistry. [1] Solventless synthesis without the use of supporting reagents which can avoid the risk of high pressure development and volatile toxic solvent employment is very amaizing and eco-friendly.

  4. An Expedient Method for the Synthesis of Thiosemicarbazones under Microwave Irradiation in Solvent-free Medium

    Institute of Scientific and Technical Information of China (English)

    LI, Jian-Ping; ZHENG, Peng-Zhi; ZHU, Jun-Ge; LIU, Rui-Jie; QU, Gui-Rong

    2006-01-01

    A simple, efficient and eco-friendly method for the synthesis of thiosemicarbazones from thiosemicarbazides and aldehyde under microwave irradiation has been reported, and no solvent and catalyst were used. And the technique of microwave irradiation coupled with solvent-free condition proved to be a quite valuable method in the organic synthesis.

  5. Silica triflate as an efficient reagent for the solvent-free synthesis of coumarins

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Silica triflate, as a new silica-based reagent, can be used for the efficient synthesis of 4-substituted coumarins via a Pechmann reaction under solvent-free reaction conditions. All reactions were performed at 80 ℃ in good to high yields.

  6. Synthesis of β3-Amino Acids via Catalyst- and Solvent-Free Aza-Michael Reaction

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A safe, environmentally friendly and cost-effective method for the synthesis of β-amino acid derivatives has been developed. Treatment of α,β-unsaturated compounds with aliphatic amines furnishes β-amino acid derivatives in good to excellent yields via a catalyst- and solvent-free aza-Michael addition.

  7. One-pot self-assembly of Cu2O/RGO composite aerogel for aqueous photocatalysis

    Science.gov (United States)

    Cai, Jingyu; Liu, Wenjun; Li, Zhaohui

    2015-12-01

    Cu2O/reduced graphene oxide (RGO) composite aerogel was fabricated by a one-pot hydrothermal method using glucose as a reducing agent and cross-linker. The as-obtained Cu2O/RGO composite aerogel showed superior photocatalytic activity for MO degradation owing to its improved light absorption capability, enhanced adsorption toward pollutant and the RGO promoted charge carrier separation. The Cu2O/RGO composite aerogel can also be facilely separated from the reaction system for recycling, which makes it especially appealing for using as a visible light responsive photocatalyst in aqueous photocatalysis.

  8. Versatility of One-pot, Single-step Synthetic Approach for Spherical Porous (Metal) Oxide Nanoparticles Using Supercritical Alcohols

    OpenAIRE

    Wang, Pengyu; Ueno, Kimiyoshi; Takigawa, Hikaru; Kobiro, Kazuya

    2013-01-01

    We developed a rapid, one-pot, single-step synthetic method for preparing spherical porous (metal) oxides, titanium dioxide, silica, zirconium dioxide, cerium dioxide, and zinc oxide with large surface areas in a supercritical alcohol containing formic acid or phthalic acid as organic additive in a very short reaction time (10 min). A new type of hollow TiO_2 nanoparticle was obtained by slowly heating the reaction mixtures. The shell thickness of hollow TiO_2 nanoparticles was controlled by ...

  9. One-pot synthesis of tetracyclic fused imidazo[1,2-a]pyridines via a three-component reaction

    Science.gov (United States)

    Yang, Bo; Tao, Chuanye; Shao, Taofeng

    2016-01-01

    Summary A novel three-component reaction has been developed to assemble biologically and pharmaceutically important tetracyclic fused imidazo[1,2-a]pyridines in a one-pot fashion utilizing readily available 2-aminopyridines, isatins and isocyanides. The three-component coupling proceeds through the Groebke–Blackburn–Bienaymé reaction followed by a retro-aza-ene reaction and subsequent nucleophilic reaction of the in-situ generated imidazo[1,2-a]pyridines bearing an isocyanate functional group. PMID:27559401

  10. Efficient one-pot synthesis of amino-benzotriazolodiazocinone scaffolds via catalyst-free tandem Ugi-Huisgen reactions.

    Science.gov (United States)

    Barlow, T M A; Jida, M; Guillemyn, K; Tourwé, D; Caveliers, V; Ballet, S

    2016-05-18

    Herein we describe a catalyst-free, one-pot procedure employing an Ugi-4CR between propargyl glycine, functionalised 2-azidoanilines, different isocyanides and aldehydes, followed by a thermal azide-alkyne Huisgen cycloaddition to generate a 14-member set of amino-benzotriazolodiazocine-bearing dipeptides with multiple points of diversification and high atom economy. These structures were derivatized by means of Suzuki-Miyaura cross-coupling reactions at two positions with good to excellent yields, leading to conformationally constrained tricyclic structures. In silico and NMR conformational analysis studies demonstrated that turn conformations are adopted by these structures. PMID:27117259

  11. One-Pot Synthesis of Biocompatible CdSe/CdS Quantum Dots and Their Applications as Fluorescent Biological Labels

    OpenAIRE

    Huang Hai; Wu Yulian; Zhai Chuanxin; Zhang Hui; Du Ning; Chen Bingdi; Yang Deren

    2011-01-01

    Abstract We developed a novel one-pot polyol approach for the synthesis of biocompatible CdSe quantum dots (QDs) using poly(acrylic acid) (PAA) as a capping ligand at 240°C. The morphological and structural characterization confirmed the formation of biocompatible and monodisperse CdSe QDs with several nanometers in size. The encapsulation of CdS thin layers on the surface of CdSe QDs (CdSe/CdS core–shell QDs) was used for passivating the defect emission (650 nm) and enhancing the ...

  12. One-pot synthesis and antifungal activity against plant pathogens of quinazolinone derivatives containing an amide moiety.

    Science.gov (United States)

    Zhang, Jin; Liu, Jia; Ma, Yangmin; Ren, Decheng; Cheng, Pei; Zhao, Jiawen; Zhang, Fan; Yao, Yuan

    2016-05-01

    An efficient one-pot, three-component synthesis of quinazolinone derivatives containing 3-acrylamino motif was carried out using CeO2 nanoparticles as catalyst. Thirty-nine synthesized compounds were obtained with satisfied yield and elucidated by spectroscopic analysis. Four phytopathogenic fungi were chosen to test the antifungal activities by minimum inhibitory concentration (MIC) method. Compounds 4ag, 4bb, 4bc showed broad antifungal activities against at least three fungi, and dramatic effects of substituents on the activities were observed. Docking studies were established to explore the potential antifungal mechanism of quinazolinone derivatives as the chitinase inhibitors, and also verified the importance of the amide moiety. PMID:27040656

  13. One-pot method of synthesis of Pt/SnO2 system and its electrocatalytic activity

    OpenAIRE

    Martyla, Agnieszka; Kopczyk, Maciej; Marciniak, Piotr; Przekop, Robert

    2014-01-01

    Background Electro-oxidation of methanol in acidic solution was investigated on a Pt/SnO2 based electrocatalyst obtained by the sol–gel method. Pt/SnO2 systems were prepared by one pot synthesis using a sol–gel method and tin (IV) acetate as a precursor of SnO2 and water solution of hexachloroplatinum acid as a source of metallic phase. Results The described method, thanks to its simplicity and mildprocessing temperature, offers uniform dispersion of metal phase in the bulk of the gel forming...

  14. A mild one-pot process for synthesising hydroxyapatite/biomolecule bone scaffolds for sustained and controlled antibiotic release

    International Nuclear Information System (INIS)

    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)

  15. One-pot hydrothermal synthesis of water-dispersible ZnS quantum dots modified with mercaptoacetic acid

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •A facile one-pot hydrothermal method to synthesize ZnS(MAA) QDs. •Synthesis and in situ modification of ZnS(MAA) QDs in a single process. •Controllable ZnS(MAA) QD size in the range 4–10 nm by varying the reaction time. •Excellent dispersibility of ZnS(MAA) QDs in water. •50% of the fluorescence signal intensity retained after storage for 6 months. -- Abstract: ZnS quantum dots (QDs) were prepared and modified in situ with mercaptoacetic acid (MAA) via a facile and environmentally friendly one-pot hydrothermal method. The resulting MAA-modified ZnS QDs (ZnS(MAA) QDs) demonstrated a cubic β-sphalerite structure, spherical morphology and controllable crystal size in the range of 4–10 nm depending on the reaction time, as characterized by X-ray diffraction, transmission electron microscopy and high-resolution transmission electron microscopy methods. The optical properties were investigated by photoluminescence spectroscopy, which showed that the fluorescence intensity increased with reaction time. After storing for 6 months, the fluorescence intensity of ZnS(MAA) QDs retained about 50% of its initial value without any peak shift

  16. One-pot electrochemical synthesis of functionalized fluorescent carbon dots and their selective sensing for mercury ion

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Yuxin; Lu, Qiujun; Deng, Jianhui; Li, Haitao; Zhang, Youyu, E-mail: zhangyy@hunnu.edu.cn

    2015-03-25

    Highlights: • One-pot electrochemical synthesis of functionalized carbon dots (C-Dots). • The C-Dots can serve as a fluorescent probe for sensitive detection of Hg{sup 2+}. • The detection limit for Hg{sup 2+} is 3.3 nM. • The sensor is successfully applied to Hg{sup 2+} determination in real samples. - Abstract: We propose a simple, economical, and one-pot method to synthesize water-soluble functionalized fluorescent carbon dots (C-Dots) through electrochemical carbonization of sodium citrate and urea. The as-prepared C-Dots have good photostability and exhibit a high quantum yield of 11.9%. The sizes of the C-Dots are mainly distributed in the range of 1.0–3.5 nm with an average size of 2.4 nm. It has been further used as a novel label-free sensing probe for selective detection of Hg{sup 2+} ions with detection limit as low as 3.3 nM. The detection linear range is 0.01–10 μM. The as-prepared C-Dots are also successfully applied for the determination of Hg{sup 2+} in real water samples.

  17. One-pot synthesis of magnetic hybrid materials based on ovoid-like carboxymethyl-cellulose/cetyltrimethylammonium-bromide templates

    International Nuclear Information System (INIS)

    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

  18. Silica-supported ionic liquid as highly efficient catalyst for one-pot synthesis of acenaphtho[1,2-]furan compounds

    Indian Academy of Sciences (India)

    Reza Sandaroos; Mohammad Taghi Goldani; Saman Damavandi

    2013-05-01

    Some new derivatives of acenaphtho[1,2-]furan have been synthesized efficiently by one-pot reaction of (acenaphthylen-1-yloxy)trimethylsilane, various aldehydes and isocyanides at the presence of silica-supported ionic liquid.

  19. T3P as an efficient cyclodehydration reagent for the one-pot synthesis of 2-amino-1,3,4-oxadiazoles

    Indian Academy of Sciences (India)

    Andivelu Ilangovan; Shanmugasundar Saravanakumar; Siddappa Umesh

    2015-05-01

    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.

  20. The Synthesis of 2,4,6-Triisopropyl-1,3,5-trioxane Catalyzed by Ionic Liquids

    Institute of Scientific and Technical Information of China (English)

    Jian Guo YANG; Xin Yu YU; Hai Hong WU; Zhi Lin CHENG; Yue Ming LIU; Ming Yuan HE

    2005-01-01

    The synthesis of 2, 4, 6-triisopropyl- 1, 3, 5-trioxane with high yield and desirable selectivity from solvent-free cyclotrimerization of isobutyraldehyde catalyzed by ionic liquids was reported in this work.

  1. 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.

  2. Solvent-free melting techniques for the preparation of lipid-based solid oral formulations.

    Science.gov (United States)

    Becker, Karin; Salar-Behzadi, Sharareh; Zimmer, Andreas

    2015-05-01

    Lipid excipients are applied for numerous purposes such as taste masking, controlled release, improvement of swallowability and moisture protection. Several melting techniques have evolved in the last decades. Common examples are melt coating, melt granulation and melt extrusion. The required equipment ranges from ordinary glass beakers for lab scale up to large machines such as fluid bed coaters, spray dryers or extruders. This allows for upscaling to pilot or production scale. Solvent free melt processing provides a cost-effective, time-saving and eco-friendly method for the food and pharmaceutical industries. This review intends to give a critical overview of the published literature on experiences, formulations and challenges and to show possibilities for future developments in this promising field. Moreover, it should serve as a guide for selecting the best excipients and manufacturing techniques for the development of a product with specific properties using solvent free melt processing.

  3. Solvent-free preparation of co-crystals of phenazine and acridine with vanillin

    International Nuclear Information System (INIS)

    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.

  4. 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.

  5. Solvent-free phase-vanishing reactions with PTFE (Teflon®) as a phase screen

    OpenAIRE

    Pels, Kevin; Dragojlovic, Veljko

    2009-01-01

    In a solvent-free phase-vanishing reaction with PTFE (polytetrafluoroethylene, Teflon®) tape as the phase screen, a thermometer adapter is utilized to insert a PTFE-sealed tube into the vapor phase above the substrate. Besides avoiding use of solvents, the experimental design is not dependent upon the densities of the reactants and the procedure generates little or no waste while providing the reaction products in high yield and in high purity.

  6. Catalyst-free and solvent-free method for the synthesis of quinoxalines under microwave irradiation

    Institute of Scientific and Technical Information of China (English)

    Jian Feng Zhou; Gui Xia Gong; Kun Bao Shi; San Jun Zhi

    2009-01-01

    A facile procedure for the synthesis.of quinoxalines is being reported starting from benzil and 1,2-diaminobenzene. Thereactions were carried out catalyst-free, solvent-free and under microwave irradiation conditions in high yield (84-98%) with short time (3-6 rain) and environmental benign, as well as convenient operation. The structures of all the compounds have been confirmed on the basis of their IR, 1H NMR, and/or 13C NMR, mass spectral data.

  7. A mild and simple synthesis of N-aryl substituted toluenesulfamides under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    ZHAO Na; WANG Yu-lu

    2004-01-01

    N- aryl substituted benzenesulfamides are often used as heating-sensitive recording material1, thermal printing material2, sensitizer3 and developer4. Moreover, some of the benzenesulfamides have antifungal activities5. Many methods have been described for preparation of sulfamides. They are used to carry out in solvent8 or in solid phase condition9. These methods required solvent or solid support and even required heating or cooling. At the same time, the process of these methods is complex. Now we have developed a new method to prepare N-aryl substituted toluenesulfamides under solvent-free conditions.In recent years, solvent-free technology has gained popularity in organic synthesis. For instance,solidstate reaction and microwave reaction have received considerable attention. Solvent-free synthesis of amides has been reported10-11. This technology has many advantages such as high efficiency and selectivity, easy separation and environmental acceptability. All these merits are in accord with green chemistry's requirements of energy-saving, high efficiency and environmental benefits.In our paper, we used a simple and efficient method for preparing N-aryl substituted toluenesulfamides under solvent-free conditions, as a replacement for classic solvent, which gives many environmental benefits.All reactions were completed at room temperature by co-grinding in an agate mortar for 3-20min and the results are shown in Table 1.In conclusion, we have developed an efficient and convenient method of preparation N-aryl substituted toluenesulfamides in high yields. It symbols an improvement for synthesis of benzenesulfamides.

  8. Structural and Morphological Properties of Cr2O3 Nanoparticles Synthesized By Novel Solvent Free Method

    OpenAIRE

    Meenambika .R; Ramalingom .S

    2014-01-01

    Nanoparticles of chromium oxide (Cr2O3) are widely used in many fields serving as catalysts, wear resistance materials, and advanced colorants. For the first time, we have reported the solvent free synthesis of Cr2O3 nanoparticles via microwave irradiation followed by calcinations at 200, 400, 600 and 800°C for 1h. The influence of calcination temperature on the particle size, microstructure and morphology was examined by X-ray diffraction, Scanning Electron Microscope (SEM) and Transmission ...

  9. Montmorillonite Clay-Promoted, Solvent-Free Cross-Aldol Condensations under Focused Microwave Irradiation

    Directory of Open Access Journals (Sweden)

    Damiano Rocchi

    2014-06-01

    Full Text Available An environmentally benign, clean and general protocol was developed for the synthesis of aryl and heteroaryl trans-chalcones. This method involved solvent-free reaction conditions under microwave irradiation in the presence of a clay-based catalyst, and afforded the target compounds in good yields and short reaction times. Furthermore, the same conditions allowed the synthesis of symmetrical, diarylmethylene-α,β-unsaturated ketones from aromatic aldehydes and ketones.

  10. An efficient synthesis of pyrazole chalcones under solvent free conditions at room temperature

    Institute of Scientific and Technical Information of China (English)

    Parvin Kumar; Sunil Kumar; Khalid Husain; Ashwani Kumar

    2011-01-01

    An easy,safe,solvent free and effective method for the synthesis of pyrazole-substituted chalcones has been achieved by grinding pyrazole aldehydes and acetophenones in the presence of activated barium hydroxide(C-200) in high yield within short span of time.All reactions were carried out just by grinding the two reactants in the presence of activated barium hydroxide(C-200).Results are also compared with sodium hydroxide and potassium hydroxide.

  11. Clean recovery of antioxidant flavonoids from onions: Optimising solvent free microwave extraction method

    OpenAIRE

    Zill-e-Huma; Vian, Maryline; Maingonnat, Jean Francois; Chemat, Farid

    2009-01-01

     A solvent free microwave hydrodiffusion and gravity extraction (MHG) of flavonol content from onion (Allium cepa L.) was studied. Effectiveness of this innovative method in extraction of onion total phenolic content, total quercetin (TQ), quercetin aglycon (QA), quercetin-3,4′-diglucoside (QDG), quercetin-4′-monoglucoside (Q4G), quercetin-3-monoglucoside (Q3G), kaempferol (KMF) and myricetin (MRT) have been evaluated and compared with conventional solvent extraction. Microwave extraction off...

  12. Solvent-free fabrication of thermally conductive insulating epoxy composites with boron nitride nanoplatelets as fillers

    OpenAIRE

    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...

  13. Controlling the Properties of Solvent-free Fe3O4 Nanofluids by Corona Structure

    Institute of Scientific and Technical Information of China (English)

    Yumo Tan; Yaping Zheng∗; Nan Wang; Aibo Zhang

    2012-01-01

    We studied the relationship between corona structure and properties of solvent-free Fe3O4 nanoflu-ids. We proposed a series of corona structures with different branched chains and synthesize different solvent-free nanofluids in order to show the effect of corona structure on the phase behavior, dispersion, as well as rheol-ogy properties. Results demonstrate novel liquid-like behaviors without solvent at room temperature. Fe3O4 magnetic nanoparticles content is bigger than 8%and its size is about 2∼3 nm. For the solvent-free nanofluids, the long chain corona has the internal plasticization, which can decrease the loss modulus of system, while the short chain of corona results in the high viscosity of nanofluids. Long alkyl chains of modifiers lead to lower viscosity and better flowability of nanofluids. The rheology and viscosity of the nanofluids are correlated to the microscopic structure of the corona, which provide an in-depth insight into the preparing nanofluids with promising applications based on their tunable and controllable physical properties.

  14. Rapid Synthesis of CoSb3/GRAPHENE Nanocomposites by One-Pot Solvothermal Route and Their Electrochemical Properties

    Science.gov (United States)

    Zheng, Yun-Xiao; Xie, Jian; Liu, Shuang-Yu; Song, Wen-Tao; Zhu, Tie-Jun; Cao, Gao-Shao; Zhao, Xin-Bing

    2012-03-01

    A facile synthetic approach for CoSb3/graphene nanocomposite has been developed in this work. By adjusting Co/Sb molar ratio, reaction temperature, and reaction time, we found that nanocrystalline CoSb3 (5-10 nm) can form at a low temperature of 180°C and a short time of only 1 h via a one-pot solvothermal route. At the same time, graphite oxide can be reduced to graphene with uniformly loaded CoSb3 nanoparticles. The composites have been characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). The nanocomposite shows improved cycling stability compared to bare CoSb3.

  15. Mesoporous C/CrN and C/VN Nanocomposites Obtained by One-Pot Soft-Templating Process

    Directory of Open Access Journals (Sweden)

    Julien Kiener

    2016-07-01

    Full Text Available Nanocomposites of ordered mesoporous carbon associated with chromium nitride (CrN or vanadium nitride (VN nanoparticles were obtained by a simple one-pot synthesis based on the solvent evaporation induced self-assembly (EISA process using Pluronic triblock surfactant as soft-template and a phenol-based resin (resol as carbon precursor. These nanocomposites were characterized by X-ray diffraction, nitrogen physisorption and Transmission Electron Microscopy (TEM techniques. Electron tomography (or 3D-TEM technique was particularly useful for providing direct insight on the internal architecture of C/CrN nanocomposite. Nanocomposites showed a very well organized hexagonal mesoporous carbon structure and a relatively high concentration of nanoparticles well distributed in the porous network. The chromium and vanadium nitrides/mesoporous carbon nanocomposites could have many potential applications in catalysis, Li-ion batteries, and supercapacitors.

  16. One-pot multiple reactions: asymmetric synthesis of 2,6-cis-disubstituted piperidine alkaloids from chiral aziridine.

    Science.gov (United States)

    Yadav, Nagendra Nath; Choi, Jihye; Ha, Hyun-Joon

    2016-07-01

    A divergent, new, and highly stereoselective synthesis of cis-2,6-disubstituted piperidine natural products including isosolenopsins, deoxocassine, and spectaline was achieved from chiral aziridine decorated with appropriate alkyl chains for isosolenopsins or alkynyl groups for deoxocassine and spectaline at C2. The characteristic feature of this synthesis is one-pot sequential reactions under atmospheric hydrogen including the reduction of alkyne (for deoxocassine and spectaline), reductive ring-opening of aziridine, debenzylation, and intramolecular reductive amination in high yields. The prerequisite aziridines were elaborated from commercially available (2S)-hydroxymethylaziridine through oxidation, Wittig olefination, and the Grignard reaction for isosolenopsins or substrate-controlled lithium alkynylate addition for deoxocassine and spectaline. PMID:27189444

  17. The first one-pot synthesis of metal-organic frameworks functionalised with two transition-metal complexes.

    Science.gov (United States)

    Platero-Prats, Ana E; Bermejo Gómez, Antonio; Samain, Louise; Zou, Xiaodong; Martín-Matute, Belén

    2015-01-01

    The synthesis of a metal-organic framework (UiO-67) functionalised simultaneously with two different transition metal complexes (Ir and Pd or Rh) through a one-pot procedure is reported for the first time. This has been achieved by an iterative modification of the synthesis parameters combined with characterisation of the resulting materials using different techniques, including X-ray absorption spectroscopy (XAS). The method also allows the first synthesis of UiO-67 with a very wide range of loadings (from 4 to 43 mol %) of an iridium complex ([IrCp*(bpydc)(Cl)Cl](2-) ; bpydc=2,2'-bipyridine-5,5'-dicarboxylate, Cp*=pentamethylcyclopentadienyl) through a pre-functionalisation methodology.

  18. One-pot synthesis of Ag nanoparticle-coated Pb-based glass frit used in crystalline silicon solar cell

    Science.gov (United States)

    Zhou, Jian; Gan, Weiping; Tang, Hongbo; Li, Yingfen; Yang, Chao

    2015-03-01

    Deposition of Ag nanoparticles onto the surface of commercial Pb-based glass frit was conducted via a novel and facile one-pot procedure—a modified polyol process. The procedure included two steps: a 5-min pretreatment of the glass frit at 25 °C in a sonication bath and a 1-h electroless plating at 75 °C in a water bath, which only involved AgNO3 and ethylene glycol but without stabilizing agent. The silver-coated glass frit particles were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, inductively coupled plasma emission spectrometer and energy dispersive spectroscopy. It was found that the glass frit particles were homogeneously coated with dense crystalline Ag nanoparticles with an average diameter of 15 nm on the surfaces. Electrical performance of the solar cells was improved after the deposition.

  19. A one-pot method to prepare N-doped titania hollow spheres with high photocatalytic activity under visible light

    Science.gov (United States)

    Ao, Yanhui; Xu, Jingjing; Zhang, Songhe; Fu, Degang

    2010-02-01

    N-doped titania hollow spheres (NTHS) were prepared by a one-pot hydrothermal method using urea as precursor of nitrogen. The prepared hollow spheres were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectrum (DRS). The photocatalytic activity of as-prepared titania hollow spheres was determined by degradation of Reactive Brilliant Red dye X-3B (C.I. reactive red 2) under visible light irradiation, and was compared to non-doped titania hollow spheres and commercial P25 titania. Results indicated that the as-prepared NTHS showed highest photocatalytic activity.

  20. One-pot synthesis of FePt/CNTs nanocomposites for efficient cellular imaging and cancer therapy

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Weihong; Zheng, Xiuwen, E-mail: xwzheng1976@163.com [Linyi University, School of Chemistry & Chemical Engineering, Shandong Provincial Key Laboratory of Detection Technology for Tumor Makers (China); Li, Shulian [Linyi Tumor Hospital (China); Zhang, Wei; Wen, Xin [Linyi University, School of Chemistry & Chemical Engineering, Shandong Provincial Key Laboratory of Detection Technology for Tumor Makers (China); Yue, Ludan [Shandong Normal University (China); Wang, Jinlong [Shandong University of Technology (China)

    2015-11-15

    Here, we developed a facile route to synthesize carbon nanotube-based FePt nanocomposites (FePt/CNTs) as a potential theranostic platform in the cancer treatment. FePt/CNTs were firstly synthesized via one-pot polyol route, and then functionalized with 6-arm-polyethylene glycol-amine polymer. The average size of FePt nanoparticles (NPs) is 3–4 nm, which is dispersed on the CNT surface (ca.50–150 nm). The as-prepared FePt NPs display high cytotoxicity by highly reactive oxygen species in cancer cells. Folic acid and fluorescein isothiocyanate are assembled onto the surface of FePt/CNTs for effective targeting of folate receptor-positive cancer cells and simultaneously for the visualization of cellular uptake. Therefore, the FePt/CNTs NPs capability of simultaneously performing diagnosis, therapy, and targeting is, therefore, promising for future potential widespread application in biomedicine.

  1. Vanillic aldehydes for the one-pot synthesis of novel 2-oxo-1,2,3,4-tetrahydropyrimidines.

    Science.gov (United States)

    Muškinja, Jovana; Janković, Nenad; Ratković, Zoran; Bogdanović, Goran; Bugarčić, Zorica

    2016-08-01

    A small library of novel 2-oxo-1,2,3,4-tetrahydropyrimidines was synthesized via a one-pot multicomponent Biginelli reaction. Copper complex [Formula: see text] which was used for the first time as a homogeneous and heterogeneous catalyst, makes this a facile and efficient reaction at room temperature. All the obtained products fall out of the solution in pure form and are easily isolated via filtration in good-to-excellent yields. The molecular structure of one of the products, ethyl 6-methyl-2-oxo-4-(4[Formula: see text]-isopropoxy-3[Formula: see text]-methoxyphenyl) - 1,2,3,4 - tetrahydropyrimidine-5- carboxylate, has been determined by X-ray crystallography. All non-hydrogen atoms in the heterocyclic, six-membered ring are determined to be approximately coplanar. PMID:26829937

  2. 缩水甘油硝酸酯的一锅法合成%One-pot Synthesis of Glycidyl Nitrate

    Institute of Scientific and Technical Information of China (English)

    邱少君; 甘孝贤; 樊慧庆

    2005-01-01

    A mild, low cost synthetic method of glycidyl nitrate is developed via so called one-pot procedure. Epichlorohydrin added dropwise to the dilute nitric acid (35 wt%) resulted in ring-opening reaction at about 20 ℃. Ring-closing occurred then by the addition of aqueous sodium hydroxide. Glycidyl nitrate was obtained in moderate yield (60%) and its structure was characterized by Fourier transform infrared spectroscopy, hydrogen and carbon nuclear magnetic resonance and elemental analysis.%环氧氯丙烷滴加到35%的稀硝酸中,于20 ℃左右进行开环反应,然后用氢氧化钠溶液进行关环反应,得到缩水甘油硝酸酯,得率为60%.用FTIR,1H NMR,13C NMR和元素分析对产物进行了结构表征.

  3. The one-pot process for the preparation of N-monoalkyl aromatic amines from nitroarene derivatives

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    A series of N-monoalkyl aromatic amines are synthesized in high yields from corresponding nitroarene derivatives,aldehydes,and ammonium formate in the presence of Pd/C as a catalyst through one-pot operations at room temperature. Both the conversion and selectivity of the process are above 80%. Optimum reaction conditions are investigated,and it is found that the optimum molar ratio of nitroarene derivatives to ammonium formate and the optimum weight ratio of nitroarene derivatives to Pd/C are 1/4 and 1/0.10,respectively. These experiments provide a novel access for N-monoalkyl aromatic amines with advantages of simplicity,high selectivity,and environmental benignity.

  4. One-pot aqueous synthesis of gadolinium doped CdTe quantum dots with dual imaging modalities.

    Science.gov (United States)

    Jiang, Chunli; Shen, Zhitao; Luo, Chunhua; Lin, Hechun; Huang, Rong; Wang, Yiting; Peng, Hui

    2016-08-01

    A facile one-pot strategy has been developed for the aqueous synthesis of Gd doped CdTe (Gd:CdTe) QDs as fluorescence and magnetic resonance imaging dual-modal agent. The prepared Gd:CdTe QDs showed narrow size distribution and the average size was less than 5nm. The amount of Gd(3+) dopant in Gd:CdTe QDs significantly affected the optical properties of obtained QDs. The highest PL QY for the prepared Gd:CdTe QDs was up to 42.5%. The QDs showed the weak toxicity and significant enhancement in MRI signal. The specific relaxivity value (r1) was determined to be 4.22mM(-1)s(-1). These properties make the prepared Gd:CdTe QDs be an effective dual-modal imaging agent and have great potential applications in biomedical field. PMID:27216651

  5. One-Pot Green Synthesis and Bioapplication of l-Arginine-Capped Superparamagnetic Fe3O4 Nanoparticles

    Science.gov (United States)

    Lai, Yongchao; Yin, Weiwei; Liu, Jinting; Xi, Rimo; Zhan, Jinhua

    2010-02-01

    Water-soluble l-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 binding l-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 the l-arginine-capped magnetite nanoparticles. The as-prepared conjugates could be used in immunomagnetic assay.

  6. 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.

  7. One-pot hydrothermal synthesis, characterization and electrochemical properties of CuS nanoparticles towards supercapacitor applications

    International Nuclear Information System (INIS)

    In this article, we have investigated the electrochemical properties of CuS nanoparticles for supercapacitor applications. The CuS nanoparticles are prepared by a facile one-pot hydrothermal approach using copper nitrate and thiourea as starting materials. The x-ray diffraction study revealed the formation of covellite CuS. The field-emission scanning electron microscope studies suggested the formation of cubic shaped CuS nanoparticles. The electrochemical studies such as cyclic voltammetry, galvanostatic charge-discharge analysis and electrochemical impedance spectroscopy confirmed the pseudocapacitive nature of the CuS electrodes. The CuS electrode shows a specific capacitance of about 101.34 F g−1 from the cyclic voltammetry at a scan rate of 5 mV s−1. The electrochemical impedance spectra analyzed using Nyquist plot confirmed the pseudocapacitive behavior of the CuS electrodes. (paper)

  8. One-pot synthesis of stable colloidal solutions of MFe2O4 nanoparticles using oleylamine as solvent and stabilizer

    International Nuclear Information System (INIS)

    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

  9. 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

    2016-01-01

    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. PMID:27098929

  10. One-pot synthesis of hydroxyapatite–silica nanopowder composite for hardness enhancement of glass ionomer cement (GIC)

    Indian Academy of Sciences (India)

    Ismail A B Rahman; Sam'an Malik Masudi; Norhayati Luddin; Rayees Ahmad Shiekh

    2014-04-01

    Hydroxyapatite–silica nanopowder composite was prepared using one-pot sol–gel technique. The morphology of the powder consists of a mixture of spherical silica particles (∼ 30 nm) embedded within the elongated hydroxyapatite (∼ 103 nm). The synthesized nanoparticles were incorporated into commercial glass ionomer cement (GIC) and Vickers hardness was evaluated. Results shown that the addition of the nanopowder composite gave ∼ 73% increment in the hardness compared to the pure GIC. Higher content of hydroxyapatite–silica nanopowder resulted in dense cement and produced a stronger GIC and the application of this material with improved hardness property might lead to extend the clinical indications, especially in stress bearing areas.

  11. MOFs as multifunctional catalysts: one-pot synthesis of menthol from citronellal over a bifunctional MIL-101 catalyst.

    Science.gov (United States)

    Cirujano, F G; Llabrés i Xamena, F X; Corma, A

    2012-04-14

    A bifunctional MOF catalyst containing coordinatively unsaturated Cr(3+) sites and palladium nanoparticles (Pd@MIL-101) has been used for the cyclization of citronellal to isopulegol and for the one-pot tandem isomerization/hydrogenation of citronellal to menthol. The MOF was found to be stable under the reaction conditions used, and the results obtained indicate that the performance of this bifunctional solid catalyst is comparable with other state-of-the-art materials for the tandem reaction: Full citronellal conversion was attained over Pd@MIL-101 in 18 h, with 86% selectivity to menthols and a diastereoselectivity of 81% to the desired (-)-menthol, while up to 30 h were necessary for attaining similar values over Ir/H-beta under analogous reaction conditions. PMID:22382815

  12. One-Pot Synthesis of Disperse Dyes Under Microwave Irradiation: Dyebath Reuse in Dyeing of Polyester Fabrics

    Directory of Open Access Journals (Sweden)

    Huda M. Mahmoud

    2012-04-01

    Full Text Available A series of 4-hydroxyphenylazopyrazolopyrimidine disperse dyes were prepared via one-pot reactions of p-hydroxyphenylhydrazone, hydrazine hydrate, and acetylacetone or enaminones using microwave irradiation as an energy source. Structural assignments of the dyes were confirmed by X-ray crystallographic structure determination. Instead of discharging the dyebath after each dyeing cycle, the residual dyebath was spectrophotometrically analyzed and then pH readjusted for a repeat dyeing with longer time. Fastness of the dyed samples was measured after each recycle. Most of the dyed fabrics tested displayed good light fastness and excellent fastness to washing and perspiration. Finally, the biological activity of the synthesized dyes against Gram positive bacteria, Gram negative bacteria and yeast were evaluated.

  13. One-pot synthesis of Fe, Co and Ni-doped carbon xerogels and their magnetic properties

    Science.gov (United States)

    Liu, Zhi; Lv, Cong; Tan, Xiuli

    2013-09-01

    Transition metal (Fe, Co and Ni)-doped carbon xerogels were synthesized by a facile one-pot pyrolysis of the sol-gel polymer of resorcinol and formaldehyde in the presence of the corresponding metal nitrates. N2 adsorption-desorption, scanning and transmission electron microscopy proved that addition of different metals could exert a remarkable influence on the textural properties. From X-ray diffraction the phases of the metallic species were identified. Scanning electron microscopy images revealed that the surface morphologies of resultant metal-carbon xerogels were composed of carbon microspheres with diameters from 5 to 15 µm. Transmission electron microscopy observations illustrated that Ni-carbon xerogel was made of uniform carbon nanotubes which differed from the approximative core/shell structures of Fe- and Co-carbon xerogels. Measurements on magnetic properties indicated that the Fe-, Co-, and Ni-carbon xerogels exhibited typical ferromagnetic characteristics at room temperature.

  14. Photothermal cancer therapy using graphitic carbon–coated magnetic particles prepared by one-pot synthesis

    Directory of Open Access Journals (Sweden)

    Lee HJ

    2014-12-01

    Full Text Available Hyo-Jeong Lee,1 Jakkid Sanetuntikul,2 Eun-Sook Choi,1 Bo Ram Lee,1 Jung-Hee Kim,1 Eunjoo Kim,1 Sangaraju Shanmugam2 1Nano and Bio Research Division, 2Department of Energy Systems Engineering, Daegu Gyeongbuk Institute of Science and Technology, Daegu, Republic of Korea Abstract: We describe here a simple synthetic strategy for the fabrication of carbon-coated Fe3O4 (Fe3O4@C particles using a single-component precursor, iron (III diethylenetriaminepentaacetic acid complex. Physicochemical analyses revealed that the core of the synthesized particles consists of ferromagnetic Fe3O4 material ranging several hundred nanometers, embedded in nitrogen-doped graphitic carbon with a thickness of ~120 nm. Because of their photothermal activity (absorption of near-infrared [NIR] light, the Fe3O4@C particles have been investigated for photothermal therapeutic applications. An example of one such application would be the use of Fe3O4@C particles in human adenocarcinoma A549 cells by means of NIR-triggered cell death. In this system, the Fe3O4@C can rapidly generate heat, causing >98% cell death within 10 minutes under 808 nm NIR laser irradiation (2.3 W cm-2. These Fe3O4@C particles provided a superior photothermal therapeutic effect by intratumoral delivery and NIR irradiation of tumor xenografts. These results demonstrate that one-pot synthesis of carbon-coated magnetic particles could provide promising materials for future clinical applications and encourage further investigation of this simple method. Keywords: graphitic carbon–encapsulated magnetic nanoparticles, iron oxide, one-pot synthesis, photothermal cancer therapy

  15. Ceric Ion Loaded MCM-41 Catalyzed Synthesis of Substituted Mono- and Bis-dihydropyrimidin-2(1H)-ones

    OpenAIRE

    Pullar Vadivel; Rathinam Ramesh; Appaswami Lalitha

    2013-01-01

    An effective one-pot three-component reaction of aromatic aldehydes with 1,3-diketone and urea or thiourea under solvent-free condition leads to the formation of mono- and bis-dihydropyrimidin-2-(1H)-ones using Ce-MCM-41 as a recyclable solid acid catalyst. This method has several advantages like simple and easy work-up with shorter reaction time, reusability of catalyst, and high yields of Biginelli products.

  16. Copper-catalyzed tandem reaction of 2-bromobenzyl bromides with 1,3-dicarbonyl compounds leading to 4H-chromenes

    Institute of Scientific and Technical Information of China (English)

    Xin Ying Zhang; Liang Liang Fang; Nan Liu; Hua Yue Wu; Xue Sen Fan

    2012-01-01

    A Cu(I)-catalyzed one-pot tandem reaction of 2-bromobenzyl bromides with 1,3-dicarbonyl compounds leading to 4H-chromene derivatives has been developed.This new approach toward 4H-chromenes combines several reactions in one pot and builds molecular complexity from readily available starting materials.

  17. Easy Access to Coumarin Derivatives Using Alumina Sulfuric Acid as an Efficient and Reusable Catalyst under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Ali Amoozadeh

    2013-01-01

    Full Text Available A new and efficient condition for the use of alumina sulfuric acid (ASA as a heterogeneous catalyst in the Pechmann condensation reaction in solvent-free condition for the formation of coumarins has been reported.

  18. SOLVENT-FREE FACILE SYNTHESIS OF NOVEL α-TOSYLOXY β-KETO SULFONES USING [HYDROXY(TOSYLOXY)IODO]BENZENE

    Science.gov (United States)

    A facile, general and high yielding protocol for the synthesis of novel α-tosyloxy β-keto sulfones is described utilizing relatively non-toxic, [hydroxy(tosyloxy)iodo]benzene, under solvent-free conditions at room temperature.

  19. Synthesis of 1, 4-Dihydropyridine Derivatives using FeCl3 as Catalyst under Solvent-free Condition

    Directory of Open Access Journals (Sweden)

    ABDORRAHMAN KEYHANI

    2013-06-01

    Full Text Available A mixture of ethyl acetoacetate, benzaldehyde and ammonium acetate and in the presence of FeCl3 under solvent-free condition were converted to 1, 4-dihydropyridines with good yields.

  20. 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

  1. 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

  2. Zinc-oxide-silica-silver nanocomposite: Unique one-pot synthesis and enhanced catalytic and anti-bacterial performance.

    Science.gov (United States)

    Kokate, Mangesh; Garadkar, Kalyanrao; Gole, Anand

    2016-12-01

    We describe herein a unique approach to synthesize zinc oxide-silica-silver (ZnO-SiO2-Ag) nanocomposite, in a simple, one-pot process. The typical process for ZnO synthesis by alkaline precipitation of zinc salts has been tweaked to replace alkali by alkaline sodium silicate. The free acid from zinc salts helps in the synthesis of silica nanoparticles, whereas the alkalinity of sodium silicate precipitates the zinc salts. Addition of silver ions into the reaction pot prior to addition of sodium silicate, and subsequent reduction by borohydride, gives additional functionality of metallic centres for catalytic applications. The synthesis strategy is based on our recent work typically involving acid-base type of cross-reactions and demonstrates a novel strategy to synthesize nanocomposites in a one-pot approach. Each component in the composite offers a unique feature. ZnO besides displaying mild catalytic and anti-bacterial behaviour is an excellent and a cheap 3-D support for heterogeneous catalysis. Silver nanoparticles enhance the catalytic & anti-bacterial properties of ZnO. Silica is an important part of the composite; which not only "glues" the two nanoparticles thereby stabilizing the nanocomposite, but also significantly enhances the surface area of the composite; which is an attractive feature of any catalyst composite. The nanocomposite is found to show excellent catalytic performance with very high turnover frequencies (TOFs) when studied for catalytic reduction of Rhodamine B (RhB) and 4-Nitrophenol (4-NP). Additionally, the composite has been tested for its anti-bacterial properties on three different bacterial strains i.e. E. coli, B. Cereus and Bacillus firmus. The mechanism for enhancement of catalytic performance has been probed by understanding the role of silica in offering accessibility to the catalyst via its porous high surface area network. The nanocomposite has been characterized by a host of different analytical techniques. The uniqueness of

  3. 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.

  4. 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. PMID:24670064

  5. Cooperative catalysis of noncompatible catalysts through compartmentalization: wacker oxidation and enzymatic reduction in a one-pot process in aqueous media.

    Science.gov (United States)

    Sato, Hirofumi; Hummel, Werner; Gröger, Harald

    2015-04-01

    A Wacker oxidation using CuCl/PdCl2 as a catalyst system was successfully combined with an enzymatic ketone reduction to convert styrene enantioselectively into 1-phenylethanol in a one-pot process, although the two reactions conducted in aqueous media are not compatible due to enzyme deactivation by Cu ions. The one-pot feasibility was achieved via compartmentalization of the reactions. Conducting the Wacker oxidation in the interior of a polydimethylsiloxane thimble enables diffusion of only the organic substrate and product into the exterior where the biotransformation takes place. Thus, the Cu ions detrimental to the enzyme are withheld from the reaction media of the biotransformation. In this one-pot process, which formally corresponds to an asymmetric hydration of alkenes, a range of 1-arylethanols were formed with high conversions and 98-99 % ee. In addition, the catalyst system of the Wacker oxidation was recycled 15 times without significant decrease in conversion. PMID:25704961

  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. 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

    2014-11-01

    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.

  8. Solvent-free Synthesis of Flavanone over New Hybrid Mesoporous Base Catalysts

    Institute of Scientific and Technical Information of China (English)

    WANG Hui; NIU Xiao-di; ZHAO Min; XIAO Xue-bin; WANG Hong-su; WANG Zhong-dong

    2011-01-01

    Benzyl and anthracenemethyl groups were respectively bonded to the N atoms of 3-aminopropyl functionalized mesoporous SBA-15(APS-SBA-15) to obtain two new base catalysts over which the condensation reaction of benzaldehyde and 2′-hydroxyacetophenone was studied.Good catalytic activities and high selectivities for flavanones were obtained in solvent-free reactions,which is attributed to the effect of benzyl and anthracenemetyl groups on the base sites of catalysts and the steric hindrance of futher reaction of flavanone with benzaldehyde.

  9. 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. PMID:25489292

  10. Organic solvents-free technique for determining sulfadimethoxine and its metabolites in chicken meat.

    Science.gov (United States)

    Furusawa, Naoto

    2007-11-16

    A quick and cost-effective technique of sample preparation followed by a reversed-phase high performance liquid chromatography under "organic solvent-free" (=100% aqueous) conditions for the simultaneous quantifying of sulfadimethoxine (SDM) and its metabolites, 6-hydroxy SDM (6-OH) and N(4)-acetyl SDM (N(4)-Ac), in chicken muscle is presented. Analysis by HPLC with photo-diode array detector was performed using a short C1 column with an isocratic 0.04 mol/l citric acid mobile phase. The method was validated by the analyses of spiked chicken muscle samples, resulting recoveries (> or =84%; relative standard deviations organic solvents were used at all.

  11. 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; De Jonghe, Joachim; 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.

  12. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance.

    Science.gov (United States)

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-01-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility. PMID:27573057

  13. 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.

  14. Smiles Rearrangement Based Practical One-pot Synthesis of N-Alkyl/aryl-6-aminoquinolines from 6-Hydroxylquinoline

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Yongsheng; Vijaykumar, B. V. D.; Jang, Kiwan; Choi, Kyungmin; Shin, Dongsoo [Changwon National Univ., Changwon (Korea, Republic of); Zuo, Hua [Southwest Univ., Chongqing (Korea, Republic of); Yoon, Yongjin [Gyeongsang National Univ., Chinju (Korea, Republic of)

    2013-12-15

    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{sub 2}CO{sub 3} or K{sub 2}CO{sub 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.

  15. 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. PMID:21615151

  16. One pot low-temperature growth of hierarchical δ-MnO2 nanosheets on nickel foam for supercapacitor applications

    International Nuclear Information System (INIS)

    Hierarchical δ-MnO2 nanosheets as electroactive materials have been directly deposited on nickel foam substrate by one-pot chelation-mediated aqueous method. The morphological evolution process has been investigated by scanning electron microscopy (SEM) at different time intervals in detail. The hierarchical δ-MnO2 electrodes which are synthesized at 30 °C, 40 °C and 50 °C are directly served as binder- and conductive-agent-free electrodes for supercapacitors and have been explored by cyclic voltammetry, galvanostatic charge-discharge test and electrochemical impedance spectroscopy. With the decrease of reaction temperature the specific capacitance of δ-MnO2 electrode increases. The vertically aligned δ-MnO2 nanosheets which have been synthesized at 30 °C exhibit a highest capacitance of 325 F g−1 at the current density of 1 A g−1. The capacitance loss is less than 15% after 1000 cycles at the scan rate of 30 mV s−1. Furthermore, it is found that the equivalent series resistance and charge transfer resistance of the electrode are 0.36 Ω and 1.7 Ω, respectively. Such superior electrochemical performance of the electrode made by directly growing porous δ-MnO2 nanosheets on nickel foam makes it has very promising applications in high-performance supercapacitors

  17. One-pot hydrothermal synthesis of an assembly of magnetite nanoneedles on a scaffold of cyclic-diphenylalanine nanorods

    International Nuclear Information System (INIS)

    The assembly of metal oxide nanoparticles (NPs) on a biomolecular template by a one-pot hydrothermal synthesis method is achieved for the first time. Magnetite (Fe3O4) nanoneedles (length: ∼100 nm; width: ∼10 nm) were assembled on cyclic-diphenylalanine (cFF) nanorods (length: 2–10 μm; width: 200 nm). The Fe3O4 nanoneedles and cFF nanorods were simultaneously synthesized from FeSO4 and l-phenylalanine by hydrothermal synthesis (220 °C and 22 MPa), respectively. The samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. Experimental results indicate that Fe3O4 nanoneedles were assembled on cFF nanorods during the hydrothermal reaction. The composite contained 3.3 wt% Fe3O4 nanoneedles without any loss of the original magnetic properties of Fe3O4.

  18. One-pot hydrothermal synthesis of an assembly of magnetite nanoneedles on a scaffold of cyclic-diphenylalanine nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Togashi, Takanari, E-mail: togashi@tagen.tohoku.ac.jp [Tohoku University, Advanced Institute for Material Research (Japan); Umetsu, Mitsuo [Tohoku University, Department of Biomolecular Engineering, Graduate School of Engineering (Japan); Naka, Takashi [National Institute for Material Science, Innovative Materials Engineering Laboratory (Japan); Ohara, Satoshi [Osaka University, Joining and Welding Research Institute (Japan); Hatakeyama, Yoshiharu [Tohoku University, Institute for Multidisciplinary for Advanced Material (Japan); Adschiri, Tadafumi [Tohoku University, Advanced Institute for Material Research (Japan)

    2011-09-15

    The assembly of metal oxide nanoparticles (NPs) on a biomolecular template by a one-pot hydrothermal synthesis method is achieved for the first time. Magnetite (Fe{sub 3}O{sub 4}) nanoneedles (length: {approx}100 nm; width: {approx}10 nm) were assembled on cyclic-diphenylalanine (cFF) nanorods (length: 2-10 {mu}m; width: 200 nm). The Fe{sub 3}O{sub 4} nanoneedles and cFF nanorods were simultaneously synthesized from FeSO{sub 4} and l-phenylalanine by hydrothermal synthesis (220 Degree-Sign C and 22 MPa), respectively. The samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. Experimental results indicate that Fe{sub 3}O{sub 4} nanoneedles were assembled on cFF nanorods during the hydrothermal reaction. The composite contained 3.3 wt% Fe{sub 3}O{sub 4} nanoneedles without any loss of the original magnetic properties of Fe{sub 3}O{sub 4}.

  19. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance

    Science.gov (United States)

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-08-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility.

  20. One-pot synthesis of hierarchical Cu2O/Cu hollow microspheres with enhanced visible-light photocatalytic activity

    Science.gov (United States)

    Hong, Tianjie; Tao, Feifei; Lin, Jiudong; Ding, Wei; Lan, Mingxuan

    2015-08-01

    The hierarchical Cu2O/Cu hollow microspheres have been fabricated by the one-pot solvothermal redox method, which is one-step approach without any surfactant and template. By using the HRTEM, XRD, XPS and UV-vis spectroscopy, the as-prepared product is composed of Cu2O and Cu with energy band gap of 1.72 eV. Based on the time-dependent experiments, the content of Cu2O and Cu compositions can be effectively controlled by adjusting the reaction time and a possible mechanism is proposed. In addition, using various dye molecules to stimulate pollutants, the hierarchical Cu2O/Cu hollow microspheres reacted for 8 h exhibit excellent visible-light photocatalytic activities, which is much higher than those of the Cu2O/Cu catalysts formed at the shorter reaction time, commercial Cu2O powder and the mixture of alone Cu2O and Cu. This enhanced photocatalytic performance makes these hierarchical Cu2O/Cu hollow microspheres a kind of efficient visible-light photocatalyst in removing some organic compounds in wastewater.

  1. One-Pot Synthesized Polyurethane-Based Nanocomposites Filled by Original Rectorite with Enhanced Strength and Elongation

    Institute of Scientific and Technical Information of China (English)

    ZHANG Fang; XIAO Zhongliang; HUANG Jin; SU Zhongnin; ZHANG Hao; ZHANG Qiaoxin

    2011-01-01

    The unmodified rectorite (REC), a kind of layered silicate, was incorporated into polyurethane (PU) as matrix by the process of one-pot synthesizing polyurethane in situ, and hence produced a series of nanocomposite materials with enhanced strength and elongation. It is worth noting that the nanocomposite containing 2 wt% REC had the maximum elongation (1 449%) and strength (32.66 Mpa) as ca. 2.7- and 1.4-fold over those of neat PU film, respectively. Meanwhile, the unexfoliated agglomerates and exfoliated nanoplatelets of REC co-existed in PU matrix. By virtue of strong interfacial interaction on the surface of REC lamella,the stress facilely transferred to the rigid RECs and hence contributed to the enhancement of strength in spite that the original structure and interaction in the PU matrix were partly cleaved. Moreover, the intertwisting of polymer chains in PU matrix with REC as well as the gliding among the REC lamellae might produce greater strain. Nevertheless, excess unexfoliated REC agglomerates under high loading level inhibited the enhancement of mechanical performances, which verified the key role of exfoliated REC nanoplatelet in improving mechanical performances. As a result, this work submitted a simple method to develop a polyurethane-based nanocomposite with high mechanical performances without any modification of layered silicates and the complicated treatment for exfoliation and dispersion.

  2. One-pot synthesis of hollow NiSe-CoSe nanoparticles with improved performance for hybrid supercapacitors

    Science.gov (United States)

    Chen, Haichao; Fan, Meiqiang; Li, Chao; Tian, Guanglei; Lv, Chunju; Chen, Da; Shu, Kangying; Jiang, Jianjun

    2016-10-01

    Hollow NiSe-CoSe samples have been synthesized for the first time via a one-pot solvothermal approach. The strategy is robust enough to synthesize NiSe-CoSe nanoparticles with different NiSe to CoSe ratios but with a similar hollow structure. Co ions in the NiSe-CoSe nanoparticles play decisive role for formation of the hollow structure; otherwise, the nanoparticles become solid for the NiSe sample. When used as the positive electroactive materials for energy storage, the NiSe-CoSe samples show excellent electrochemical activity in alkaline electrolyte. Using the synergistic effect between NiSe and CoSe, the electrochemical performance of NiSe-CoSe can be tuned by varying the NiSe to CoSe ratios. The NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 shows the best electrochemical performance in terms of superior specific capacity, improved rate capability and excellent cycling stability. In addition, the electrochemical performance of NiSe-CoSe sample with a NiSe to CoSe ratio of 4:2 is also evaluated via assembling hybrid supercapacitors with RGO, and the hybrid supercapacitor delivers both high power and energy densities (41.8 Wh kg-1 at 750 W kg-1 and 20.3 Wh kg-1 at 30 kW kg-1).

  3. One-Pot Terpolymerization of CO2, Propylene Oxide and Lac- tide Using Rare-earth Ternary Catalyst

    Institute of Scientific and Technical Information of China (English)

    顾林; 秦玉升; 高永刚; 王献红; 王佛松

    2012-01-01

    A convenient one-pot terpolymerization of CO2, propylene oxide (PO), and L-lactide (L-LA) in short polymerization time (10 h or shorter) to afford poly(propylene carbonate-lactide) with excellent mechanical property and thermal stability using Y(CCl3COO)3-ZnEtz-glycerin rare-earth ternary catalyst is reported. The yield of the co- polymerization was between 69.7 and 111.7 g/(g Zn), corresponding to L-LA/PO molar feed ratio varying from 0 to 0.1, and the number average molecular weight was between 5.5×10^4 and 11.9 × 10^4. The L-LA content in the ter- polymer increased from 1.1% to 34.7% when L-LA/PO molar feed ratio changed from 0.01 to 0.1. Introducing L-LA as the third comonomer could significantly improve the mechanical strength and thermal stability of PPC. For the terpolymer obtained from L-LA/PO molar feed ratio of 1:50, the elongation at break reached 40.5%, which is 3 times of that of pure PPC, and the thermal decomposition temperature increased by 32℃ compared with pure PPC.

  4. One-pot synthesis of interpenetrating inorganic/organic networks of CuO/resorcinol-formaldehyde aerogels: nanostructured energetic materials.

    Science.gov (United States)

    Leventis, Nicholas; Chandrasekaran, Naveen; Sadekar, Anand G; Sotiriou-Leventis, Chariklia; Lu, Hongbing

    2009-04-01

    For many applications ranging from catalysis to sensors to energetic materials, it is desirable to produce intimate mixtures of nanoparticles. For instance, to improve the reaction rates of energetic materials, the oxidizing agent and the fuel need to be mixed as intimately as possible, ideally at the nanoscopic level. In this context, the acidity of a hydrated CuCl(2) solution reacting toward a network of CuO nanoparticles (a good oxidant) is used to induce one-pot cogelation of a nanostructured network of a resorcinol-formaldehyde resin (RF, the fuel). The resulting wet gels are dried to aerogels, and upon pyrolysis under Ar, the interpenetrating CuO/RF network undergoes a smelting reaction toward metallic Cu. Upon ignition in the open air, pure RF aerogels do not burn, while CuO/RF composites, even with substoichiometric CuO, sustain combustion, burning completely leaving only a solid residue of CuO whose role then has been that of a redox mediator through the smelting reaction.

  5. One-Pot Synthesis of SnO2/C Nanocapsules Composites as Anode Materials for Lithium-Ion Batteries.

    Science.gov (United States)

    Yang, Lina; Chen, Kexun; Dong, Tao; Wang, Zhao; Li, Guomin; Zhang, Yanling; Zhang, Lipeng

    2016-02-01

    In this work, we demonstrate a facile route for the synthesis of nanostructured SnO2/C composites for lithium-ion batteries. The anode materials were prepared via a one-pot solvothermal approach and then calcination in a highly pure nitrogen atmosphere. The composited was composed of amor- phous carbon and nanocrystalline SnO2 by the X-ray diffraction (XRD) analysis, and the content of carbon was calculated according to the thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) images revealed that the diameter of these as-prepared spheres varied from 50 to 60 nm. A systematic study has been carried out to examine the effect of carbon content upon lithium-ion battery performance. The electrochemical results showed that SnO2/C nanocomposite could achieve 1197.5 mAh/g reversible capacity and 55.11% initial coulombic efficiency, and 190% capacity retention after 50 cycles compared to the SnO2 nanoparticles of 940.6 mAh/g at a current density 0.2 C in the voltage range of 0.01-3.0 V. These improvements can be ascribed to the carbon, which can enhance the conductivity of SnO2, suppress the aggregation of active particles, and increase their structural stability during cycling. PMID:27433668

  6. One-pot template-free synthesis of porous CdMoO4 microspheres and their enhanced photocatalytic activity

    Science.gov (United States)

    Madhusudan, Puttaswamy; Zhang, Jinfeng; Yu, Jiaguo; Cheng, Bei; Xu, Difa; Zhang, Jun

    2016-11-01

    The optical and catalytic performances of materials strongly depend on their size, morphology, dimensionality and structure. Herein, we demonstrate a facile one-pot template free synthesis of hierarchical CdMoO4 porous microspheres via a simple low temperature oil bath method. The photoactivity of the as-prepared samples was evaluated by photocatalytic decolorization of Methyl Orange (MO) and Methylene Blue (MB) mixed dye aqueous solutions at ambient temperature under full solar spectrum. The results indicated that the concentration of ammonium molybdate and reaction time greatly influence the diameter, average crystallite size, specific surface area, pore structure and photocatalytic activity of the prepared samples. Especially, under the suitable conditions the prepared hierarchical CdMoO porous microspheres exhibited enhanced photocatalytic activity and high stability. Furthermore, it is found that the photocatalytic activity and formation rate of hydroxyl radicals greatly depend on the particle sizes and morphology of as-prepared samples. This work not only demonstrates a simple way to fabricate the hierarchical CdMoO4 porous microspheres but also shows a possibility for utilization of CdMoO4 porous microspheres for the photocatalytic treatment of waste water pollutants.

  7. A Facile One-Pot Synthesis of Au/Cu2O Nanocomposites for Nonenzymatic Detection of Hydrogen Peroxide

    Science.gov (United States)

    Chen, Ting; Tian, Liangliang; Chen, Yuan; Liu, Bitao; Zhang, Jin

    2015-06-01

    Au/Cu2O nanocomposites were successfully synthesized by a facile one-pot redox reaction without additional reducing agent under room temperature. The morphologies and structures of the as-prepared products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The electrocatalytic performance of Au/Cu2O nanocomposites towards hydrogen peroxide was evaluated by cyclic voltammetry (CV) and chronoamperometry (CA). The prepared Au/Cu2O nanocomposite electrode showed a wide linear range from 25 to 11.2 mM ( R = 0.9989) with a low detection limit of 1.05 μM ( S/ N = 3) and high sensitivity of 292.89 mA mM-1 cm-2. The enhanced performance for H2O2 detection can be attributed to the introduction of Au and the synergistic effect between Au and Cu2O. It is demonstrated that the Au/Cu2O nanocomposites material could be a promising candidate for H2O2 detection.

  8. One-Pot Synthesis of Biocompatible CdSe/CdS Quantum Dots and Their Applications as Fluorescent Biological Labels

    Directory of Open Access Journals (Sweden)

    Huang Hai

    2011-01-01

    Full Text Available Abstract We developed a novel one-pot polyol approach for the synthesis of biocompatible CdSe quantum dots (QDs using poly(acrylic acid (PAA as a capping ligand at 240°C. The morphological and structural characterization confirmed the formation of biocompatible and monodisperse CdSe QDs with several nanometers in size. The encapsulation of CdS thin layers on the surface of CdSe QDs (CdSe/CdS core–shell QDs was used for passivating the defect emission (650 nm and enhancing the fluorescent quantum yields up to 30% of band-to-band emission (530–600 nm. Moreover, the PL emission peak of CdSe/CdS core–shell QDs could be tuned from 530 to 600 nm by the size of CdSe core. The as-prepared CdSe/CdS core–shell QDs with small size, well water solubility, good monodispersity, and bright PL emission showed high performance as fluorescent cell labels in vitro. The viability of QDs-labeled 293T cells was evaluated using a 3-(4,5-dimethylthiazol-2-diphenyltertrazolium bromide (MTT assay. The results showed the satisfactory (>80% biocompatibility of as-synthesized PAA-capped QDs at the Cd concentration of 15 μg/ml.

  9. One-pot synthesis of stable water soluble Mn:ZnSe/ZnS core/shell quantum dots

    International Nuclear Information System (INIS)

    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 H2O2 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 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.

  11. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor.

    Science.gov (United States)

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    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. PMID:26901204

  12. One-pot preparation and CO2 adsorption modeling of porous carbon, metal oxide, and hybrid beads.

    Science.gov (United States)

    Drisko, Glenna L; Aquino, Cindy; Feron, Paul H M; Caruso, Rachel A; Harrisson, Simon; Luca, Vittorio

    2013-06-12

    Hierarchically porous carbon (C), metal oxide (ZrTi), or carbon-metal oxide (CZrTi) hybrid beads are synthesized in one pot through the in situ self-assembly of Pluronic F127, titanium and zirconium propoxides, and polyacrylonitrile (PAN). Upon contact with water, a precipitation of PAN from the liquid phase occurs concurrently with polymerization and phase separation of the inorganic precursors. The C, ZrTi, and CZrTi materials have similar morphologies but different surface chemistries. The adsorption of carbon dioxide by each material has been studied and modeled using the Langmuir-Freundlich equation, generating parameters that are used to calculate the surface affinity distributions. The Langmuir, Freundlich, Tóth, and Temkin models were also applied but gave inferior fits, indicating that the adsorption occurred on an inhomogeneous surface reaching a maximum capacity as available surface sites became saturated. The carbon beads have higher surface affinity for CO2 than the hybrid and metal oxide materials. PMID:23672249

  13. A Facile Route for Patterned Growth of Metal-Insulator Carbon Lateral Junction through One-Pot Synthesis.

    Science.gov (United States)

    Park, Beomjin; Park, Jaesung; Son, Jin Gyeong; Kim, Yong-Jin; Yu, Seong Uk; Park, Hyo Ju; Chae, Dong-Hun; Byun, Jinseok; Jeon, Gumhye; Huh, Sung; Lee, Seoung-Ki; Mishchenko, Artem; Hyun, Seung; Lee, Tae Geol; Han, Sang Woo; Ahn, Jong-Hyun; Lee, Zonghoon; Hwang, Chanyong; Novoselov, Konstantin S; Kim, Kwang S; Hong, Byung Hee; Kim, Jin Kon

    2015-08-25

    Precise graphene patterning is of critical importance for tailor-made and sophisticated two-dimensional nanoelectronic and optical devices. However, graphene-based heterostructures have been grown by delicate multistep chemical vapor deposition methods, limiting preparation of versatile heterostructures. Here, we report one-pot synthesis of graphene/amorphous carbon (a-C) heterostructures from a solid source of polystyrene via selective photo-cross-linking process. Graphene is successfully grown from neat polystyrene regions, while patterned cross-linked polystyrene regions turn into a-C because of a large difference in their thermal stability. Since the electrical resistance of a-C is at least 2 orders of magnitude higher than that for graphene, the charge transport in graphene/a-C heterostructure occurs through the graphene region. Measurement of the quantum Hall effect in graphene/a-C lateral heterostructures clearly confirms the reliable quality of graphene and well-defined graphene/a-C interface. The direct synthesis of patterned graphene from polymer pattern could be further exploited to prepare versatile heterostructures. PMID:26144549

  14. 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

  15. PhI(OAc)2-mediated one-pot oxidative decarboxylation and aromatization of tetrahydro-β-carbolines: synthesis of norharmane, harmane, eudistomin U and eudistomin I.

    Science.gov (United States)

    Kamal, Ahmed; Tangella, Yellaiah; Manasa, Kesari Lakshmi; Sathish, Manda; Srinivasulu, Vunnam; Chetna, Jadala; Alarifi, Abdullah

    2015-08-28

    Iodobenzene diacetate was employed as a mild and efficient reagent for one-pot oxidative decarboxylation of tetrahydro-β-carboline acids and dehydrogenation of tetrahydro-β-carbolines to access the corresponding aromatic β-carbolines. To the best of our knowledge this is the first synthesis of β-carbolines via a one-pot oxidative decarboxylation at ambient temperature. The utility of this protocol has been demonstrated in the synthesis of β-carboline alkaloids norharmane (2o), harmane (2p), eudistomin U (9) and eudistomin I (12). PMID:26099113

  16. High surface area nanocrystalline hausmannite synthesized by a solvent-free route

    International Nuclear Information System (INIS)

    Highlights: ► High surface area Mn3O4 nanoparticles obtained by a solvent-free low temperature route. ► 3,6,9-Trioxadecanoic acid allows to obtain nanocrystalline hausmannite. ► Tape casted electrodes show up to 300 mAh g−1 capacity after more than 40 cycles at a C/3 rate. ► Upper cut off voltage strongly influences capacity retention upon cycling at high C rates. -- Abstract: Nanocrystalline high surface area Mn3O4 powder was obtained at low temperature by a solvent-free route. The precursor was a mixture of manganese (II) acetate, 3,6,9-trioxadecanoic acid (TODA) and ammonium acetate that were intimately mixed by grounding in an agate mortar. Nanocrystalline Mn3O4 was obtained by thermal treatment at 120 °C. Powder X-ray diffraction, selected area electron diffraction, high resolution transmission electron microscopy, and Fourier transformed infrared characterization confirmed the formation of the hausmannite phase. The as-prepared mesoporous material has high specific surface area (120 m2 g−1). The performances of tape casted Mn3O4 nanopowder electrodes were investigated as anode material for lithium ion batteries. High capacity values were achieved at diverse C rates. Capacity fading was found to be dependent on the upper cut off voltage, the presence of a plateau at 2.25 V vs. Li+/Li being detrimental for long term cyclability.

  17. 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.

  18. Ruthenium-Catalyzed Olefin Metathesis after Tetra-n-butylammonium Fluoride-Mediated Desilylation

    Science.gov (United States)

    Osman, Sami

    2012-01-01

    One-pot procedures expedite organic synthesis but pose challenges in that many reagents must be compatible with each other. We discovered that the presence of nBu4NF hindered rutheniumcatalyzed olefin metathesis when nBu4NF-mediated desilylation and olefin metathesis were performed in one pot. This problem could be solved by the addition of (TMS)2O to remove fluoride anions in order to facilitate the ruthenium-catalyzed olefin metathesis. PMID:23269856

  19. Self-assembled one-pot synthesis of red luminescent CdS:Mn/Mn(OH)2 nanoparticles

    International Nuclear Information System (INIS)

    We report a novel method of growing red luminescent (635 nm) Mn-doped CdS (CdS:Mn) nanoparticles capped by an inorganic shell of Mn(OH)2. CdSO4, Na2S2O3 and Mn(NO3)2 were used as the precursors, and thioglycerol (C3H8O2S) was employed as the capping agent and also the catalyst of the reaction. Using these materials resulted in very slow rate of the reaction and particles growth. The self-assembled one-pot process was performed at pH of 8 and Mn:Cd ratio of 10, and took about 10 days for completion. CdS:Mn nanoparticles are slowly formed in the first day of the process; however, the luminescence is weak. After 7 days, the solution turns white turbid through the formation of additional particles, which precipitate on the walls on the next day. At this stage, a relatively strong red luminescence at 635 nm appears from transparent solution of the CdS:Mn nanoparticles. The white deposit on the walls turns to dark-brown color and luminescence increases on the 9th day. Finally, the CdS:Mn nanoparticles agglomerate and precipitate out of the solution on 10th day. X-ray diffraction and optical spectroscopy showed crystalline phase CdS nanoparticles with an average size of 3.6 nm. We explain the luminescence enhancement based on the formation of a Mn(OH)2 shell on the surface of the CdS:Mn nanoparticles during the precipitation stage. This can passivate the S dangling bonds located on the particles surface. As the surface Cd sites are previously capped with thioglycerol molecules, a complete surface passivation is achieved and results in emergence of high-intensity luminescence

  20. One-pot preparation of new copolymer electrolytes with tunable network structure for all-solid-state lithium battery

    Science.gov (United States)

    Chen, Bo; Xu, Qiang; Huang, Zhen; Zhao, Yanran; Chen, Shaojie; Xu, Xiaoxiong

    2016-11-01

    A new class of copolymer electrolytes with tunable network structure is successfully designed and prepared via a facile one-pot reaction. The trimethylolpropane triglycidyl ether (TMPEG) is cross-linked with poly (ethylene glycol) diamine (NPEG) to create well-defined solid network polymer electrolyte (SNPE). The network structure could be tuned by changing the molar ratio of TMPEG and NPEG or the molecular weight of NPEG. The effects of molecular weight of NPEG and molar ratio of EO/Li+ on the ionic conductivity are systematically investigated. The optimal electrolyte TMPEG-NPEG4K[2:1]-16:1 presents a maximum conductivity of 1.10 × 10-4 S cm-1 under 30 °C, and an 18-fold ionic conductivity enhancement in that of PEO-based electrolyte. Furthermore, it also exhibits wide electrochemical window (0-5.4 V), excellent compatibility with metallic Li, and superior mechanical properties. The all-solid-state lithium batteries LiFePO4/Li are assembled with TMPEG-NPEG4K[2:1]-16:1 electrolyte, and present good cycling and rate performance under 60 °C. The initial discharge specific capacities of the batteries are 161.7 mAh g-1 at 0.2 C and 132.7 mAh g-1 at 1 C, and the capacity retention ratio can be retained at 90.6% and 90.5% after 100 cycles. This new copolymer electrolyte may become a promising candidate for applications in all-solid-state lithium battery.

  1. 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.

  2. One-pot room temperature synthesizing Cu- and Mn-doped ZnSe nanocrystals by a rapid photochemical method

    Science.gov (United States)

    Bahador, A. R.; Molaei, M.; Karimipour, M.

    2016-04-01

    In this work, a one-pot, rapid, green and room temperature photochemical synthesis of transition metal (TM; Cu, Mn)-doped ZnSe nanocrystals (NCs) was reported. NCs were successfully characterized using Fourier transform-infrared (FT-IR), photoluminescence (PL) and UV-Visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), X-ray diffractometry (XRD) and energy dispersive X-ray spectra (EDX). FT-IR spectra confirmed the capping of ZnSe by thioglycolic acid (TGA) molecules. XRD and TEM analysis demonstrated zinc blend phase NCs with an average size of around 3 nm. Band gap of ZnSe NCs was about 3.6 eV which it was decreased by increasing the illumination time. PL spectra of ZnSe NCs showed a broad emission with two peaks located at 380 nm and 490 nm related to excitonic and trap states emission, respectively. For ZnSe:Cu NCs, excitonic emission disappeared completely and PL intensity of trap states emission increased with the increase in the Cu2+ ion concentration so that for precursor ratio of Cu:Zn 1%, optimal value of PL intensity was obtained. For ZnSe:Mn NCs, the excitonic emission decreased gradually with the increase in the impurity concentration whereas trap state emission increased. Moreover, a peak about 590 nm was appeared from 4T1-6A1 transition of the Mn2+ impurity, demonstrating the Mn incorporation inside the ZnSe NCs structure.

  3. 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.

  4. One-pot and Three-Component Synthesis of isoxazol-5(4H-one Derivatives in the presence of Citric Acid

    Directory of Open Access Journals (Sweden)

    Ashkan bashash Rikani

    2016-06-01

    Full Text Available In this context, the one-pot three-component synthesis of 3-methyl-4-arylmethylene-isoxazol-5(4H-ones has been performed in the presence of citric acid as catalyst in water. The products have been obtained in high yields (70-90% and convenient reaction times (5-24 hours.

  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. Novel and efficient one-pot five- and six-component reactions for the stereoselective synthesis of highly functionalized enaminones and dithiocarbamates.

    Science.gov (United States)

    Bararjanian, Morteza; Balalaie, Saeed; Rominger, Frank; Movassagh, Barahman; Bijanzadeh, Hamid Reza

    2011-05-01

    Efficient methods for stereoselective synthesis of polyfunctional (E)-enaminones and (Z)-dithiocarbamates via one-pot five- and six-component sequential Ugi/Nucleophilic addition reactions are described. High yields and high bond forming efficiency, and simple operations are the advantages of this method. PMID:21072590

  8. A facile and convenient approach for the one-pot synthesis of 2,4(1H,3H)-quinazolinediones

    Institute of Scientific and Technical Information of China (English)

    Mahnaz Sharafi-Kolkeshvandi; Farzad Nikpour

    2012-01-01

    A fast and efficient method is described for the one-pot synthesis of 2,4(1H,3H)-quinazolinediones by cyclization reaction of anthranilic acid derivatives with potassium cyanate and acetic acid in PEG.Good to high yields of the products obtain in short reaction times with simple work-up.

  9. One-Pot Synthesis of Benzo[4,5]imidazo[2,1-a]isoquinolines and Isoquinolino[3,4-b]quinoxalines via Tandem Cyclization Strategies.

    Science.gov (United States)

    Bagdasarian, Alex L; Nguyen, Huy H; Palazzo, Teresa A; Fettinger, James C; Haddadin, Makhluf J; Kurth, Mark J

    2016-05-01

    Two operationally simple one-pot protocols have been developed for the synthesis of amino-functionalized benzo[4,5]imidazo[2,1-a]isoquinolines and isoquinolino[3,4-b]quinoxalines. Optimization data and substrate scope for these atom-economical transformations, which engage commercially available o-phenylenediamines and o-cyanobenzaldehydes, are discussed. PMID:27030441

  10. 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.

  11. Development of one-pot three component reaction for the synthesis of N′-aryl-N-cyanoformamidines, essential precursors of formamidine pesticides family

    Directory of Open Access Journals (Sweden)

    Antonio De Nino

    2016-01-01

    Full Text Available Efficient one-pot three component reaction of aniline derivatives with cyanoamide and triethyl orthoformate at reflux in toluene affords N′-aryl-N-cyanoformamidines in high yields just by the distillation of the azeotrope toluene/ethyl alcohol. Labelled d9-Amitraz is prepared by the application of this procedure in the synthesis of formamidine pesticides family.

  12. Expedient access to α,β-difunctionalized azepenes using α-halo eneformamides: application to the one-pot synthesis of 2-benzazepanes.

    Science.gov (United States)

    Bassler, Daniel P; Spence, Laura; Alwali, Amir; Beale, Oliver; Beng, Timothy K

    2015-02-28

    The regioselective synthesis of α,β-difunctionalized (alkenyl, aryl, sulfonyl, allyl, or alkynyl) azepenes has been accomplished through α-halo eneformamides. A successful implementation of the vicinal functionalization strategy has led to a one-pot synthesis of 2-benzazepanes whose benzenoid portion is highly functionalized.

  13. 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

  14. Dual response surface-optimized synthesis of L-menthyl conjugated linoleate in solvent-free system by Candida rugosa lipase.

    Science.gov (United States)

    Li, Zhen; Wang, Yulun; Li, Jia; Wang, Ping; Wei, Wei; Gao, Yang; Fu, Chenyin; Dong, Wenqi

    2010-02-01

    Lipase-catalyzed synthesis of L-menthyl conjugated linoleate in solvent-free system was studied in this paper. Duel response surface methodology was employed to explore the factors which would influence the reaction conversion by a range of independent experiments. The conditions of reaction temperature, reaction time, enzyme amount, substrate molar ratio and water content were symmetrically investigated. When the substrates were 1 mmol CLA and 1 mmol L-menthol, the maximum conversion (79.1+/-0.8%) was obtained at 30 degrees C, Candida rugosa lipase of 33.7% (w/w by weight of L-menthol), water content of 32% (w/w by weight of L-menthol), reaction time of 43 h. The product isomers (9Z,11E-/10E,12Z-=63/37) were analyzed by GC/MS. The similarity between the oleic acid and 9Z,11E-CLA conformations which were obtained by molecular modeling could account for the specific catalyzed by C. rugosa lipase. PMID:19833506

  15. A highly efficient procedure for the oxathioacetalization of carbonyl compounds under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The novel efficient procedure has been developed for the oxathioacetalization of carbonyl compounds and 2-mercaptoethanol using the novel carbon-based sulfonic acid as catalyst under solvent-free condition at room temperature. The results showed that the novel catalyst was very efficient for the reactions with good to excellent yields in short time. The novel catalyst owned many advantages such as operational simplicity,without need of any solvent,small amount of usage,low cost of the catalyst used,high yields,applicability to large-scale reactions,reusability and chemoselectivity over the traditional catalysts,which made the catalyst one of the best choices for the reactions.

  16. 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.

  17. A Mild and Efficient Synthesis of Benzimidazole by Using Zinc Chloride under Solvent Free Condition

    Directory of Open Access Journals (Sweden)

    Mahajan Tushar

    2013-02-01

    Full Text Available A straightforward, efficient and more sustainable solvent-free method has been developed for the synthesis of benzimidazole derivatives to achieve yields that were comparable to or better than, those in conventional media. It is noteworthy that the reaction was exclusively carried out in Zinc chloride catalysis system, rendering the methodology highly valuable from both environment and economic points of view. The various benzimidazoles were synthesized by the reaction of o-phenylenediamine with different types of aldehydes and characterized by their Physical constant, FT-IR Spectra, 1H NMR Spectra and LCMS. The excellent chemo selectivity, mild reaction condition, short reaction times and excellent yield made the best method then other methods.

  18. A novel carbon-14 'solvent-free'-labeling procedure with diethyl malonate

    International Nuclear Information System (INIS)

    A novel labelling procedure for dialkyl malonate preparation under 'solvent-free' conditions in the presence of a phase transfer catalyst was developed. Improved radiochemical yields (about 70%) as compared to the classical preparation routes in DMF are achieved in mere 10 minutes at 130 deg C. General labelling procedures for alkyl bromides are reported. The radiochemical purity by HPLC and analysis conditions using online radioactivity detection are described. The preparation of radiochemicals by this method shows major advantages as regards the purification of the final labelled compound and, since no organic solvent is used, waste management. A simple and easy two-step chromatographic procedure gives rise to pure dialkyl malonates. The method can be especially useful in short-lived isotope labelling

  19. Olive oil glycero lysis with the immobilized lipase Candida antarctica in a solvent free system

    Energy Technology Data Exchange (ETDEWEB)

    Singh, A. K.; Mukhopadhyay, M.

    2012-11-01

    In the present work, the solvent free lipase glycerolysis of olive oil for the production of monoglyceride (MG) and diglyceride (DG) with an immobilized Lipase B Candida antarctica was studied. The experiments were performed in batch mode by varying different process parameters. The Results showed that the MG and DG yields were dependent on operating conditions such as time, temperature, glycerol/ oil molar ratio, enzyme concentration and the water content in glycerol. The optimum operating time for maximum MG, 26 wt% and DG, 30 wt% production was 3h. The initial reaction rate was studied by varying different process parameters for 1h. The initial reaction rate increased at 30 degree centigrade temperature, 2:1 glycerol/oil molar ratio, 3.5% (w/w) water content in glycerol and 0.015g of enzyme loading. Comparative data for MG and DG yields for different oils and enzyme combinations were presented.

  20. 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)

  1. Lipase coated clusters of iron oxide nanoparticles for biodiesel synthesis in a solvent free medium.

    Science.gov (United States)

    Mukherjee, Joyeeta; Gupta, Munishwar Nath

    2016-06-01

    Methyl or ethyl esters of long chain fatty acids are called biodiesel. Biodiesel is synthesized by the alcoholysis of oils/fats. In this work, lipase from Thermomyces lanuginosus was precipitated over the clusters of Fe3O4 nanoparticles. This biocatalyst preparation was used for obtaining biodiesel from soybean oil. After optimization of both immobilization conditions and process parameters, complete conversion to biodiesel was obtained in 3h and on lowering the enzyme amount, as little as 1.7U of lipase gave 96% conversion in 7h. The solvent free media with oil:ethanol (w/w) of 1:4 and 40°C with 2% (w/w) water along with 20% (w/w) silica (for facilitating acyl migration) were employed for reaching this high % of conversion. The biocatalyst design enables one to use a rather small amount of lipase. This should help in switching over to a biobased production of biodiesel. PMID:26967340

  2. 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.

  3. 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.

  4. One-pot facile electrospinning construct of flexible Janus nanofibers with tunable and enhanced magnetism–photoluminescence bifunctionality

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Liyan [Jilin Jianzhu University, Key Laboratory of Building Energy-Saving Technology Engineering, College of Materials Science and Engineering (China); Dong, Xiangting, E-mail: dongxiangting888@163.com [Changchun University of Science and Technology, Key Laboratory of Applied Chemistry and Nanotechnology at Universities of Jilin Province (China); Gai, Guangqing, E-mail: gaigq@163.com; Zhao, Li [Jilin Jianzhu University, Key Laboratory of Building Energy-Saving Technology Engineering, College of Materials Science and Engineering (China); Xu, Shuzhi [Jilin Business and Technology College, School of Biotechnology Engineering (China); Xiao, Xinfu [Jilin Jianzhu University, Key Laboratory of Building Energy-Saving Technology Engineering, College of Materials Science and Engineering (China)

    2015-02-15

    A novel nanostructure of flexible Janus nanofibers with tunable and enhanced magnetism–photoluminescence difunctionality has been successfully fabricated by one-pot electrospinning using specially designed parallel spinneret. Europium complex Eu(BA){sub 3}phen (BA = benzoic acid, phen = 1,10-phenanthroline), terbium complex Tb(BA){sub 3}phen, and Fe{sub 3}O{sub 4} nanoparticles (NPs) were, respectively, incorporated into polyvinyl pyrrolidone (PVP) and electrospun into Janus nanofibers. The morphology, structure, and property of the Janus nanofibers were investigated in detail by scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, fluorescence spectroscopy, and vibrating sample magnetometry. The average diameter of the Janus nanofibers is about ca. 300 nm. Every Janus nanofiber is composed of one nanofiber with different performances on two sides, one side is composed of Fe{sub 3}O{sub 4} NPs and PVP, and the other side consists of [Eu(BA){sub 3}phen + Tb(BA){sub 3}phen] and PVP. This novel nanostructures can effectively isolate Eu(BA){sub 3}phen and Tb(BA){sub 3}phen from Fe{sub 3}O{sub 4} NPs so that the exciting light and emitting light in the [Eu(BA){sub 3}phen + Tb(BA){sub 3}phen]/PVP domain will almost not be affected by Fe{sub 3}O{sub 4} NPs. The Janus nanofibers possess higher fluorescent intensity owing to their special nanostructure compared with non-Janus composite nanofiber with the same compositions. Moreover, the Janus nanofibers have multicolored and color-tunable photoluminescence, the emitting color could be tuned in a wide color range of red–yellow–green by adjusting the molar ratio of Eu(BA){sub 3}phen to Tb(BA){sub 3}phen under the excitation of 274-nm single-wavelength ultraviolet light, and the magnetism also could be tuned by changing the amounts of Fe{sub 3}O{sub 4} NPs. The new type Janus nanofibers with tunable and enhanced magnetism–photoluminescence bifunctionality have

  5. 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.

  6. Cu-Catalyzed Multicomponent Reaction of Styrenes, Perfluoroalkyl Halide, Alcohol, and tert-Butyl Hydroperoxide: One-Pot Synthesis of (Z)-β-Alkoxyperfluoroalkenone.

    Science.gov (United States)

    Luo, Qiang; Liu, Chunmei; Tong, Jingjing; Shao, Ying; Shan, Wenyu; Wang, Hanghang; Zheng, Hao; Cheng, Jiang; Wan, Xiaobing

    2016-04-15

    An efficient synthesis of Z-perfluoroalkyl-substituted enones by a multicomponent reaction strategy has been described. A variety of elusive perfluoroalkylated enones are furnished under mild reaction conditions in good yields with unique chemo- and stereoselectivity. A sequence of radical-mediated Kornblum-DeLaMare reaction, Michael addition, and HF elimination is proposed for the mechanism. PMID:26980724

  7. One-pot three-component synthesis of tetrahydrobenzo[b]pyrans catalyzed by cost-effective ionic liquid in aqueous medium☆

    Institute of Scientific and Technical Information of China (English)

    Jianguo Yang; Shuo Liu; Huanan Hu; Shibin Ren; Anguo Ying

    2015-01-01

    A simple and efficient method is proposed for the synthesis of tetrahydrobenzo[b]pyrans with aromatic alde-hydes, active methylene compounds, and dimedone using basic ionic liquid catalyst in water. The procedure offers several advantages including short reaction time, good yield, easy procedure, and good recyclability of catalysts, which may be a practical alternative to conventional processes for preparation of 4-hpyrans.

  8. Ferric Perchlorate Catalyzed One-pot Synthesis of 1,2,3,4-Tetrahydro-2-pyrimidinones and -thiones:an Expedient Protocol for the Biginelli Reaction

    Institute of Scientific and Technical Information of China (English)

    HERAVI,Majid Momahed; BEHBAHANI,Farahnaz Kargar OSKOOIE; Hossien Abdi

    2008-01-01

    An efficient synthesis of 1,2,3,4-tetrahydro-2-pyrimidinones and -thiones using ferric perchlorate as the catalyst from an aldehyde, ethyl acetoacetate, and urea or thiourea in acetonitrile was described. Compared to the classical Biginelli reaction conditions, this new method consistently has the advantage of full catalysis, good yields and short reaction time.

  9. 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.

    ) and some indolo[2,3-b]quinolines (3a–d) against human hepatocellular carcinoma HepG2 and human breast carcinoma MCF-7 cells. Anti-proliferative assay against human hepatocellular carcinoma HepG2 and human breast carcinoma MCF-7 cells indicated methyl...

  10. Optimization of technological conditions for one-pot synthesis of (S)-α-cyano-3-phenoxybenzyl acetate in organic media

    Institute of Scientific and Technical Information of China (English)

    ZHANG Ting-zhou; YANG Li-rong; ZHU Zi-qiang

    2005-01-01

    Optically active form of α-cyano-3-phenoxybenzyl (CPB) alcohol, building block of pyrethroid insecticides, was synthesized as its acetate by the combination of anion-exchange resin (D301)-catalyzed transcyanation between m-phenoxybenzaldehyde (m-PBA) and acetone cyanohydrin (AC), and lipase (from Alcaligenes sp.)-catalyzed enantioselective transesterification of the resulting cyanohydrin with vinyl acetate. Through optimizing technological conditions, the catalyzing efficiency was improved considerably compared to methods previously reported. Concentrations of CPB acetate were determined by gas chromatograph. The enantio excess (e.e.) values of CPB acetate were measured by NMR (nuclear magnetic resonance) method. Effects of solvents and temperatures on this reaction were studied. Cyclohexane was shown to be the best solvent among the three tested solvents. 55 ℃ was the optimal temperature for higher degree of conversion. External diffusion limitation was excluded by raising the rotational speed to 220 r/min. However, internal diffusion could not be ignored, since the catalyst (lipase) was an immobilized enzyme and its particle dimension was not made small enough. The reaction rate was substantially accelerated when the reactant (m-PBA) concentration was as high as 249 mmol/L, but decreased when the initial concentration of m-PBA reached to 277 mmol/L. It was also found that the catalyzing capability of recovered lipase was high enough to use several batches. Study of the mole ratio of AC to m-PBA showed that 2:1 was the best choice. The strategy of adding base catalyst D301 was found to be an important factor in improving the degree of conversion of the reaction from 20% to 80%. The highest degree of conversion of the reaction has reached up to 80%.

  11. A polymer surfactant corona dynamically replaces water in solvent-free protein liquids and ensures macromolecular flexibility and activity.

    Science.gov (United States)

    Gallat, François-Xavier; Brogan, Alex P S; Fichou, Yann; McGrath, Nina; Moulin, Martine; Härtlein, Michael; Combet, Jérôme; Wuttke, Joachim; Mann, Stephen; Zaccai, Giuseppe; Jackson, Colin J; Perriman, Adam W; Weik, Martin

    2012-08-15

    The observation of biological activity in solvent-free protein-polymer surfactant hybrids challenges the view of aqueous and nonaqueous solvents being unique promoters of protein dynamics linked to function. Here, we combine elastic incoherent neutron scattering and specific deuterium labeling to separately study protein and polymer motions in solvent-free hybrids. Myoglobin motions within the hybrid are found to closely resemble those of a hydrated protein, and motions of the polymer surfactant coating are similar to those of the hydration water, leading to the conclusion that the polymer surfactant coating plasticizes protein structures in a way similar to hydration water.

  12. Kinetics of carrier-mediated ion transport in two new types of solvent-free lipid bilayers.

    OpenAIRE

    Lapointe, J Y; Laprade, R

    1982-01-01

    In contrast with the usual glyceryl-monooleate/decane (GMO-D) bilayer lipid membranes, new membranes, formed from a mixture of GMO in squalene (GMO-S) or from a mixture of GMO in triolein (GMO-T), seem to be almost solvent free. Our results from voltage-jump relaxation studies, using these "solvent-free" membranes with the homologue carriers, nonactin, monactin, dinactin, trinactin, and tetranactin, are compared with the corresponding ones for GMO-D membranes. With all homologues, solvent-fre...

  13. PbO as an efficient and reusable catalyst for one-pot synthesis of tetrahydro benzo pyrans and benzylidene malonitriles

    Indian Academy of Sciences (India)

    Ashok V Borhade; Bhagwat K Uphade; Dipak R Tope

    2013-05-01

    PbO nanoparticles have been employed as an efficient catalyst for the solvent-free synthesis of tetrahydrobenzo pyrans (yields 81-91%) and benzylidene malonitriles (yields 90-96%) at room temperature using green chemistry approach. PbO nanoparticles were found to be highly efficient, eco-friendly and recyclable heterogeneous catalyst. PbO nanoparticles were prepared by hydrothermal method and characterized by IR, XRD, BET Surface area, SEM, EDAX and TEM with SAED techniques.

  14. A facile one-pot hydrothermal method to prepare europium-doped titania hollow phosphors and their sensitized luminescence properties

    Energy Technology Data Exchange (ETDEWEB)

    Feng Xuan; Yang Ling; Zhang Nianchun [Department of Chemistry and Institute of Nanochemistry, Jinan University, 601 Western Huangpu Road, Guangzhou 510632 (China); Liu Yingliang, E-mail: tliuyl@jnu.edu.c [Department of Chemistry and Institute of Nanochemistry, Jinan University, 601 Western Huangpu Road, Guangzhou 510632 (China)

    2010-09-17

    Research highlights: {yields} The strongest emission intensity was observed with TiO{sub 2}:Eu{sub 0.2} hollow spheres and TiO{sub 2}:Eu{sub 0.2} hollow spheres calcining at 550 {sup o}C. Moreover, the strongest excitation of TiO{sub 2}:Eu{sub 0.2} hollow spheres transferred from 400 to 500 {sup o}C and the effective nonradiative energy transfer from the TiO{sub 2} hollow spheres host matrix to Eu{sup 3+} ions crystal field states was realized due to changes of crystalline field in the environment around Eu{sup 3+} ions occupying Ti{sup 4+} sites. The proposed energy transfer mechanism was that UV light is absorbed in the band of TiO{sub 2} hollow spheres crystal and then the energy is relaxed to the defect states of TiO{sub 2} host. The energy can transfer to the crystal states of Eu{sup 3+} ions ({sup 7}F{sub j}, j = 0, 1, 2, 3 and 4), which results in efficient photoluminescence. The fluorescent intensity of TiO{sub 2}:Eu{sub 0.2} hollow spheres was 2.2 times as strong as that of TiO{sub 2}:Eu{sub 0.2} bulk material. - Abstract: Monodisperse europium-activated titania hollow phosphors had been synthesized by a facile one-pot hydrothermal method using carbon spheres as hard templates. Samples were characterized by X-ray powder diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, energy dispersive spectrometer and photoluminescence spectrum. The strongest emission intensity was observed with TiO{sub 2}:Eu{sub 0.2} hollow spheres and TiO{sub 2}:Eu{sub 0.2} hollow spheres calcining at 550 {sup o}C. Moreover, the strongest excitation of TiO{sub 2}:Eu{sub 0.2} hollow spheres transferred from 400 to 500 {sup o}C and the effective nonradiative energy transfer from the TiO{sub 2} hollow spheres host matrix to Eu{sup 3+} ions crystal field states was realized due to changes of crystalline field in the environment around Eu{sup 3+} ions occupying Ti{sup 4+} sites. The proposed energy transfer mechanism was that UV light is absorbed in the band

  15. Manganese dioxide mediated one-pot synthesis of methyl 9H-pyrido[3,4-b]indole-1-carboxylate: Concise synthesis of alangiobussinine

    Directory of Open Access Journals (Sweden)

    Jessica Baiget

    2011-10-01

    Full Text Available The carboline ring system is an important pharmacophore found in a number of biologically important targets. Development of synthetic routes for the preparation of these compounds is important in order to prepare a range of analogues containing the carboline heterocyclic moiety. A manganese dioxide mediated one-pot method starting with an activated alcohol and consisting of alcohol oxidation, Pictet–Spengler cyclisation, and oxidative aromatisation, offers a convenient process that allows access to β-carbolines. This one-pot process for the preparation of methyl 9H-pyrido[3,4-b]indole-1-carboxylate has subsequently been used as the key step in the synthesis of alangiobussinine and a closely related analogue.

  16. BF₃·OEt₂ mediated metal-free one-pot sequential multiple annulation cascade (SMAC) synthesis of complex and diverse tetrahydroisoquinoline fused hybrid molecules.

    Science.gov (United States)

    Shinde, Anand H; Vidyacharan, Shinde; Sharada, Duddu S

    2016-03-28

    A highly efficient and distinct BF3·OEt2 mediated metal-free SMAC protocol for the synthesis of complex and diverse hybrid molecules viz. indazole fused tetrahydroisoquinolinoquinoxalines, and tetrahydroisoquinolinodiazepine has been developed. The transformation is based on sequential cascade processes involving 2H-indazole formation and deprotection Pictet-Spengler cyclization steps in one-pot fashion. The protocol demonstrates the utility of sequential multiple annulations in a cascade fashion. The present one-pot protocol uses the Solid State Melt Reaction (SSMR) strategy for the synthesis of the intermediate 2H-indazole. The method is operationally simple and represents a new approach for C-C, three C-N and N-N bond formation with a wide substrate scope. PMID:26935814

  17. One-Pot Synthesis of Organic-Sulfur-Zinc Hybrid Materials via Polycondensation of a Zinc Salt and Thiols Generated in Situ from Cyclic Dithiocarbonates.

    Science.gov (United States)

    Ochiai, Bungo; Konta, Hirohisa

    2015-08-17

    Soluble organic-sulfur-zinc hybrid polymers were prepared via a one-pot reaction consisting of ring-opening addition and subsequent polycondensation. The first reaction is the nucleophilic ring-opening addition of 2-ethylhexylamine to multifunctional cyclic dithiocarbonates giving multiple thiols in situ. The sequential polycondensation of the in situ generated thiols with Zn(OAc)2 gave the target hybrid polymers. This one-pot method enabled the use of a shorter amine than the previous polycondensation of Zn(OAc)2 and purified thiols, which required octadecylamine to obtain a soluble product. The obtained hybrid polymers may be cast as composite films with polystyrene and poly(methyl methacrylate). Owing to the shorter alkyl chain, the calculated nD values of the products (1.60 or 1.61) are higher than that of the previous product bearing octadecyl chains (1.53).

  18. One-Pot Synthesis of Organic-Sulfur-Zinc Hybrid Materials via Polycondensation of a Zinc Salt and Thiols Generated in Situ from Cyclic Dithiocarbonates

    Directory of Open Access Journals (Sweden)

    Bungo Ochiai

    2015-08-01

    Full Text Available Soluble organic-sulfur-zinc hybrid polymers were prepared via a one-pot reaction consisting of ring-opening addition and subsequent polycondensation. The first reaction is the nucleophilic ring-opening addition of 2-ethylhexylamine to multifunctional cyclic dithiocarbonates giving multiple thiols in situ. The sequential polycondensation of the in situ generated thiols with Zn(OAc2 gave the target hybrid polymers. This one-pot method enabled the use of a shorter amine than the previous polycondensation of Zn(OAc2 and purified thiols, which required octadecylamine to obtain a soluble product. The obtained hybrid polymers may be cast as composite films with polystyrene and poly(methyl methacrylate. Owing to the shorter alkyl chain, the calculated nD values of the products (1.60 or 1.61 are higher than that of the previous product bearing octadecyl chains (1.53.

  19. Excellent performance of one-pot synthesized Cu-SSZ-13 catalyst for the selective catalytic reduction of NOx with NH3.

    Science.gov (United States)

    Xie, Lijuan; Liu, Fudong; Ren, Limin; Shi, Xiaoyan; Xiao, Feng-Shou; He, Hong

    2014-01-01

    Cu-SSZ-13 samples prepared by a novel one-pot synthesis method achieved excellent NH3-SCR performance and high N2 selectivity from 150 to 550 °C after ion exchange treatments. The selected Cu3.8-SSZ-13 catalyst was highly resistant to large space velocity (800 000 h(-1)) and also maintained high NOx conversion in the presence of CO2, H2O, and C3H6 in the simulated diesel exhaust. Isolated Cu(2+) ions located in three different sites were responsible for its excellent NH3-SCR activity. Primary results suggest that the one-pot synthesized Cu-SSZ-13 catalyst is a promising candidate as an NH3-SCR catalyst for the NOx abatement from diesel vehicles. PMID:24295053

  20. SiO2-Diphenic acid: An efficient and recyclable heterogeneous catalyst for one-pot synthesis of bis-(indolyl)methane derivatives in liquid phase

    Indian Academy of Sciences (India)

    R Vaid; M Gupta; O S Chambyal; R Gupta

    2015-06-01

    An eco-friendly and expedient procedure for one-pot synthesis of is-(indolyl)methane derivatives via electrophilic substitution reaction at C-3 position of indole with various aldehydes has been developed by using silica-diphenic acid as a novel heterogeneous catalyst. This method has various promising features such as short reaction time, easy work-up procedure, good yield of products and remarkable activity and selectivity of the catalyst.

  1. 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.

  2. An efficient one-pot three-component synthesis of tetrahydrobenzo[b]pyran and 3,4-dihydropyrano[c]chromene derivatives using starch solution as catalyst

    Institute of Scientific and Technical Information of China (English)

    Nourallah Hazeri; Malek Taher Maghsoodlou; Fatemeh Mir; Mehrnoosh Kangani; Hamideh Saravani; Ebrahim Molashahi

    2014-01-01

    Tetrahydrobenzo[b]pyran and 3,4-dihydropyrano[c]chromene derivatives were synthesized via a one-pot three-component condensation of aromatic aldehydes with malononitrile and dimedone or 4-hydroxycoumarin in excellent yields in the presence of starch solution as a highly efficient ho-mogenous catalyst. The use of a nontoxic and biodegradable catalyst, simple work-up procedure, and short reaction time are advantages of this method.

  3. A one-pot hydrothermal synthesis of sulfur and nitrogen doped carbon aerogels with enhanced electrocatalytic activity in the oxygen reduction reaction

    OpenAIRE

    Wohlgemuth, Stephanie-Angelika; White, Robin Jeremy; Willinger, Marc-Georg; Titirici, Maria-Magdalena; Antonietti, Markus

    2012-01-01

    A one-pot, hydrothermal synthesis of nitrogen and sulfur dual doped carbon aerogels is presented, derived from our previously published hydrothermal carbonization approach. Two co-monomers, S-(2-thienyl)-L-cysteine (TC) and 2-thienyl carboxaldehyde (TCA), were used for sulfur incorporation, giving rise to distinct morphologies and varying doping levels of sulfur. Nitrogen-doping levels of 5 wt% and sulfur-doping levels of 1 wt% (using TCA) to 4 wt% (using TC) were obtained. A secondary pyroly...

  4. Solid-supported sulfonic acid-containing catalysts efficiently promoted one-pot multi-component synthesis of -acetamido carbonyl compounds

    Indian Academy of Sciences (India)

    Mohammad Ali Zolfigol; Ardeshir Khazaei; Abdolkarim Zare; Mohammad Mokhlesi; Tahereh Hekmat-Zadeh; Alireza Hasaninejad; Fatemeh Derakhshan-Panah; Ahmad Reza Moosavi-Zare; Hassan Keypour; Ahmad Ali Dehghani-Firouzabadid; Maria Merajoddin

    2012-03-01

    Silica-functionalized sulfonic acid (SFSA) and sulfuric acid-modified polyethylene glycol-6000 (PEG-OSO3H) efficiently catalysed one-pot multi-component condensation of enolizable ketones or alkyl acetoacetates with arylaldehydes, acetonitrile and acetyl chloride to afford the corresponding -acetamido ketone or ester derivatives in high to excellent yields and in relatively short reaction times. Moreover, in this work, some novel -acetamido carbonyl compounds (i.e., one complex structure) are synthesized.

  5. Baylis-Hillman acetates in organic synthesis: convenient one-pot synthesis of α-carboline framework--a concise synthesis of neocryptolepine.

    Science.gov (United States)

    Basavaiah, Deevi; Mallikarjuna Reddy, Daggula

    2012-11-28

    A convenient, facile, and one-pot methodology for the synthesis of α-carbolines from Baylis-Hillman (BH) acetates, involving three steps (reactions), (1) mono alkylation of 2-nitroarylacetonitriles with BH-acetates, (2) reduction of nitro group into amino group using Fe/AcOH and (3) formation of two (five and six membered) rings, is presented. This methodology is successfully applied to the synthesis of bioactive alkaloid neocryptolepine.

  6. Facile synthesis of 1H-imidazo[1,2-b]pyrazoles via a sequential one-pot synthetic approach

    OpenAIRE

    Demjén, András; Gyuris, Márió; Wölfling, János; Puskás, László G.; Kanizsai, Iván

    2014-01-01

    5-Aminopyrazole-4-carbonitrile and ethyl 5-aminopyrazole-4-carboxylate, as potential trifunctional building blocks are introduced in a facile, chemo- and regioselective multicomponent assembly of imidazo[1,2-b]pyrazoles via the Groebke–Blackburn–Bienaymé reaction (GBB reaction). Besides the synthetic elaboration of a green-compatible isocyanide-based access in three-component mode, we describe an operationally simple, one-pot two-step GBB protocol for the rapid construction of a 46 membered i...

  7. Facile synthesis of 1H-imidazo[1,2-b]pyrazoles via a sequential one-pot synthetic approach

    OpenAIRE

    András Demjén; Márió Gyuris; János Wölfling; Puskás, László G.; Iván Kanizsai

    2014-01-01

    5-Aminopyrazole-4-carbonitrile and ethyl 5-aminopyrazole-4-carboxylate, as potential trifunctional building blocks are introduced in a facile, chemo- and regioselective multicomponent assembly of imidazo[1,2-b]pyrazoles via the Groebke–Blackburn–Bienaymé reaction (GBB reaction). Besides the synthetic elaboration of a green-compatible isocyanide-based access in three-component mode, we describe an operationally simple, one-pot two-step GBB protocol for the rapid construction of a 46 membered i...

  8. 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.

  9. One-pot synthesis of novel pyrimido[4,5-]quinolines and pyrido[2,3-:6,5']dipyrimidines using encapsulated--Fe2O3 nanoparticles

    Indian Academy of Sciences (India)

    Moona Mohsenimehr; Manouchehr Mamaghani; Farhad Shirini; Mehdi Sheykhan; Sima Abbaspour; Leila Shafei Sabet

    2015-11-01

    Novel pyrimido[4,5-]quinolines and pyrido[2,3-:6,5-']dipyrimidine derivatives were synthe-sized in one-pot, three-component approach using sulfonic acid supported on hydroxyapatite-encapsulated--Fe2O3 [-Fe2O3 @HAp-SO3H] as magnetically recoverable nanocatalyst. The protocol provided a rapid, useful and green method for the preparation of the products in short reaction times and high yields.

  10. Nano copper and cobalt ferrites as heterogeneous catalysts for the one-pot synthesis of 2,4,5-tri substituted imidazoles

    Indian Academy of Sciences (India)

    Paul Douglas Sanasi; D Santhipriya; Y Ramesh; M Ravi Kumar; B Swathi; K Jaya Rao

    2014-11-01

    A simple one-pot synthesis has been developed for the synthesis of 2,4,5-trisubstituted imidazoles using magnetic recyclable spinel nano copper and cobalt ferrites by the condensation of benzil, aromatic aldehyde and ammonium acetate in ethanol as solvent. The reaction, with these catalysts was carried out under mild reaction conditions with very good yields of substituted imidazoles. These catalysts can be recycled very easily and reused, which makes this methodology environmentally benign.

  11. Synthesis of a Library of 1,5,2-Dithiazepine 1,1-Dioxides. Part 1: A One-Pot Sulfonylation/Thia-Michael Protocol

    Science.gov (United States)

    Zang, Qin; Zhou, Aihua; Javed, Salim; Maity, Pradip K.; Knudtson, Chris A.; Bi, Danse; Hastings, Jared J.; Basha, Fatima Z.; Hanson, Paul R.

    2013-01-01

    A novel one-pot sulfonylation/intramolecular thia-Michael protocol is reported for the synthesis of 1,5,2-dithiazepine 1,1-dioxides. Sulfonylation between cysteine ethyl ester/cysteamine and 2-chloroethanesulfonyl chloride, followed by in situ intramolecular thia-Michael addition, was achieved and afforded the titled 1,5,2-dithiazepine-1,1-dioxide scaffolds. Diversification was demonstrated for future library synthesis. PMID:24385679

  12. One pot production of 5-hydroxymethylfurfural with high yield from cellulose by a Brønsted-Lewis-surfactant-combined heteropolyacid catalyst.

    Science.gov (United States)

    Zhao, Shun; Cheng, Mingxing; Li, Junzi; Tian, Juan; Wang, Xiaohong

    2011-02-21

    A Brønsted-Lewis-surfactant-combined heteropolyacid (HPA) Cr[(DS)H(2)PW(12)O(40)](3) has been synthesized, and is used as a heterogeneous catalyst for the conversion of cellulose to 5-hydroxymethylfurfural in one pot within 2 h at 150 °C with 77.1% conversion and 52.7% yield. This micellar HPA catalyst shows stability and can be recycled by simple separation process. PMID:21203610

  13. One-Pot Synthesis of (NiFe2O4)x-(SrFe12O19)1-x Nanocomposites and Their Microwave Absorption Properties.

    Science.gov (United States)

    Hazra, Subhenjit; Ghosh, Barun Kumar; Patra, Manoj Kumar; Jani, Raj Kumar; Vadera, Sampat Raj; Ghosh, Narendra Nath

    2015-09-01

    In this paper, we report a simple but novel aqueous solution based 'one-pot' method for preparation of (NiFe2O4)x-(SrFe12O19)1-x nanocomposites consist of hard ferrite-soft ferrite phases. A physical mixing method has also been employed to prepare nanocomposites having same compositions. The effects of synthetic methodologies on the microstructures of the nanocomposites as well as their magnetic and microwave absorption properties have been evaluated. Crystal structures and microstructures of these composites have been investigated by using X-ray diffraction, transmission electron microscope and scanning electron microscope. In the nanocomposites, prepared by both methods, presence of nanocrystalline NiFe2O4 and SrFe12O19 phases was detected. However, nanocomposites, prepared by one-pot method, possessed better homogeneous distribution of hard and soft ferrite phases than the nanocomposites, prepared by physical mixing method. Nanocomposites, prepared by one-pot method, demonstrated significant spring exchange coupling interaction between hard and soft ferrite phases and exhibited magnetically single phase behaviour. The spring exchange coupling interaction enhanced the magnetic properties (high saturation magnetization and coercivity) and microwave absorption properties of the nanocomposites, prepared by one-pot method, in comparison with the nanocomposites prepared by physical mixing method as well as pure NiFe2O4 and SrFe12O19 nanoparticles. Minimum reflection loss of the composite was ~ -17 dB (i.e., 98% absorption) at 8.2 GHz for an absorber thickness of 3.2 mm. PMID:26716212

  14. Methods for synthesizing diethyl carbonate from ethanol and supercritical carbon dioxide by one-pot or two-step reactions in the presence of potassium carbonate

    OpenAIRE

    Gasc, Fabien; Thiebaud-Roux, Sophie; Mouloungui, Zephirin

    2009-01-01

    Carbon dioxide sequestration was studied by synthesizing diethyl carbonate (DEC) from ethanol and CO2 under supercritical conditions in the presence of potassium carbonate as a base. The co-reagent was ethyl iodide or a concentrated strong acid. This sequestration reaction occurs in two steps, which were studied separately and in a one-pot reaction. An organic-inorganic carbonate hybrid, potassium ethyl carbonate (PEC) is generated at the end of the first step. This intermediate was character...

  15. 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.

  16. Microwave-assisted synthesis of new N4-[bi-(4-fluorophenyl)-methyl]-piperazine thiosemicarbazones under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Qing Han Li; Zhi Gang Zhao

    2008-01-01

    Six new N4-[bi-(4-fluorophenyl)-methyl]-piperazine thiosemicarbazones 3a-f have been prepared starting from [bi-(4-fluor-ophenyl)-methyl]-piperazine in solvent-free condition under microwave irradiation with excellent yields. Their structures have been determined by elemental analysis, IR, MS and 1H NMR data.

  17. Synthesis of naphthoxazinone derivatives using silica-bonded -sulfonic acid as catalyst under solvent-free conditions

    Indian Academy of Sciences (India)

    Khodabakhsh Niknam; Parisa Abolpour

    2015-07-01

    Silica-bonded -sulfonic acid is employed as a recyclable catalyst for the synthesis of naphthoxazinone derivatives from the reaction of -naphthol, aromatic aldehydes and urea at 150°C under solvent-free conditions. The heterogeneous catalyst was recycled for five runs after the reaction of -naphthol, benzaldehyde and urea without losing its catalytic activity.

  18. 21 CFR 182.40 - Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings.

    Science.gov (United States)

    2010-04-01

    ... conjunction with spices, seasonings, and flavorings. 182.40 Section 182.40 Food and Drugs FOOD AND DRUG... in conjunction with spices, seasonings, and flavorings. Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings that are generally recognized as safe for their...

  19. An expendient method for the synthesis of bis(acylhydrazones) under microwave irradiation in solvent-free medium

    Energy Technology Data Exchange (ETDEWEB)

    Li, J.P.; Zheng, P.Z.; Zhu, J.G.; Liu, R.J.; Qu, G.R. [Henan Normal University, Xinxiang (China). College of Chemical and Environmental Science. Key Lab. of Environmental Pollution Control Technology of Henan Province]. E-mail: jplig@163.com

    2007-10-15

    A simple, efficient and eco-friendly method for the synthesis of bis(acylhydrazones) from hexanediohydrazide and aldehydes under microwave irradiation without the use of solvent and catalyst is reported. The technique of microwave irradiation under solvent-free condition proved to be quite a valuable method in organic synthesis. (author)

  20. Solvent-free Synthesis of Dihydrofuran-fused [60]Fullerene Derivatives by High-speed Vibration Milling

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Solvent-free reactions of 1, 3-cyclohexanedione, 5, 5-dimethyl-1, 3-cyclohexanedione,ammonium nitrate (CAN) under the high-speed vibration milling conditions afforded dihydrofuran-fused C60 derivatives. CAN is the better oxidant than Mn(OAc)3.2H2O in these mechanochemical reactions.

  1. K-10 clay as a reusable catalyst for the solvent-free MW-induced synthesis of enaminones

    Directory of Open Access Journals (Sweden)

    Marvi Omid

    2014-01-01

    Full Text Available A series of β-amino-α, β-unsaturated ketones and esters synthesized from the reaction of different amines with 1,3- dicarbonyl compounds in solvent-free media using montmorillonite K-10 clay as solid recyclable heterogeneous acidic catalyst and microwave irradiation in good to excellent yields.

  2. Environmentally benign synthesis of sydnone containing 1,3,4-thiadiazines under microwave and solvent-free conditions

    Indian Academy of Sciences (India)

    Jyoti C Hegde; Satheesha Rai N; Balakrishna Kalluraya

    2007-07-01

    Novel, convenient and benign synthesis of 2-arylamino-5-(3'-arylsydnone-4-yl)-1,3,4-thiadiazines 3a-l by the interaction of 3-substituted-4-bromoacetyl sydnones 1 with substituted thiosemicarbazides 2 under MW irradiation and solvent-free condition is described.

  3. A Solvent-free Approach to Glycosyl Amides: Towards the Synthesis of α-N-Galactosyl Ceramides

    Science.gov (United States)

    Chennamadhavuni, Divya; Howell, Amy R.

    2015-01-01

    A new, simple and efficient method for the synthesis of both α- and β-glycosyl amides using solvent-free conditions is described. This method involves the coupling of glycosyl amines with the p-nitrophenol esters of lipids as a key step. PMID:26028787

  4. Mg(ClO4)2 catalysed preparation of 1-amidoalkyl-2-naphthols under solvent-free conditions

    Indian Academy of Sciences (India)

    Mohammad Ali Amrollahi; Bi Bi Fatemeh Mirjalili; Hamideh Emtiazi

    2013-05-01

    A simple, efficient, and practical procedure for the synthesis of amidoalkyl naphthols via multicomponent one-pot reaction of 2-naphthol, aldehydes and amides catalysed by Mg(ClO4)2 is described in high yields. The present work offers several advantages such as high

  5. One-Pot Synthesis of Graphene-Supported Monodisperse Pd Nanoparticles as Catalyst for Formic Acid Electro-oxidation

    Science.gov (United States)

    Yang, Sudong; Dong, Jing; Yao, Zhaohui; Shen, Chengmin; Shi, Xuezhao; Tian, Yuan; Lin, Shaoxiong; Zhang, Xiaogang

    2014-03-01

    To synthesize monodisperse palladium nanoparticles dispersed on reduced graphene oxide (RGO) sheets, we have developed an easy and scalable solvothermal reduction method from an organic solution system. The RGO-supported palladium nanoparticles with a diameter of 3.8 nm are synthesized in N-methyl-2-pyrrolidone (NMP) and in the presence of oleylamine and trioctylphosphine, which facilitates simultaneous reduction of graphene oxide and formation of Pd nanocrystals. So-produced Pd/RGO was tested for potential use as electrocatalyst for the electro-oxidation of formic acid. Pd/RGO catalyzes formic acid oxidation very well compared to Pd/Vulcan XC-72 catalyst. This synthesis method is a new way to prepare excellent electrocatalysts, which is of great significance in energy-related catalysis.

  6. 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.

  7. Reactions of Organic Ions at Ambient Surfaces in a Solvent-Free Environment

    Science.gov (United States)

    Badu-Tawiah, Abraham K.; Cyriac, Jobin; Cooks, R. Graham

    2012-05-01

    Solvent-free ion/surface chemistry is studied at atmospheric pressure, specifically pyrylium cations, are reacted at ambient surfaces with organic amines to generate pyridinium ions. The dry reagent ions were generated by electrospraying a solution of the organic salt and passing the resulting electrosprayed droplets pneumatically through a heated metal drying tube. The dry ions were then passed through an electric field in air to separate the cations from anions and direct the cations onto a gold substrate coated with an amine. This nontraditional way of manipulating polyatomic ions has provided new chemical insights, for example, the surface reaction involving dry isolated 2,4,6-triphenylpyrylium cations and condensed solid-phase ethanolamine was found to produce the expected N-substituted pyridinium product ion via a pseudobase intermediate in a regiospecific fashion. In solution however, ethanolamine was observed to react through its N-centered and O-centered nucleophilic groups to generate two isomeric products via 2H-pyran intermediates. The O-centered nucleophile reacted less rapidly to give the minor product. The surface reaction product was characterized in situ by surface enhanced Raman spectroscopy, and ex situ using mass spectrometry and H/D exchange, and found to be chemically the same as the major pyridinium solution-phase reaction product.

  8. A Diazonium Salt-Based Ionic Liquid for Solvent-FreeModification of Carbon.

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Chengdu [ORNL; Huang, Jing-Fang [ORNL; Li, Zuojiang [ORNL; Luo, Huimin [ORNL; Dai, Sheng [ORNL

    2006-01-01

    A novel ionic liquid that consists of p-butylbenzenediazonium ions and bis(trifluoromethanesulfonyl)amidates (Tf{sub 2}N{sup -}) has been synthesized as a task-specific ionic liquid for the solvent-free modification of carbon materials. The use of anions Tf{sub 2}N{sup =} is the key to rendering the hydrophobicity, low liquidus temperature, and ionicity to this novel molten salt. This diazonium salt has a melting point of 7.2 C and a moderate electric conductivity of 527 {micro} s/cm at 25 C. The thermal stability of this diazonium ionic liquid has been investigated by high-resolution thermogravimetric analysis (HRTGA). The compound is stable up to about 90 C in nitrogen, which is only 10 C less than its solid tetrafluoroborate counterpart. The modification of carbon materials has been carried out through both thermal and electrochemical activations of diazonium ions to generate free radical intermediates without the use of any solvent. The surface-coverage loadings of 3.38 {micro} mol/m{sup 2} and 6.07 {micro} mol/m{sup 2} for covalently attached organic functionalities have been achieved by the thermally induced functionalization and electrochemically assisted reaction, respectively.

  9. Self-assembling dipeptides: conformational sampling in solvent-free coarse-grained simulation.

    Science.gov (United States)

    Villa, Alessandra; Peter, Christine; van der Vegt, Nico F A

    2009-03-28

    We discuss the development of a coarse-grained (CG) model for molecular dynamics (MD) simulation of a hydrophobic dipeptide, diphenylalanine, in aqueous solution. The peptide backbone is described with two CG beads per amino acid, the side groups and charged end groups are each described with one CG bead. In the derivation of interaction functions between CG beads we follow a bottom-up strategy where we devise potentials such that the resulting CG simulation reproduces the conformational sampling and the intermolecular interactions observed in an atomistic simulation of the same peptide. In the CG model, conformational flexibility of the peptide is accounted for through a set of intra-molecular (bonded) potentials. The approach followed to obtain the bonded potentials is discussed in detail. The CG potentials for nonbonded interactions are based on potentials of mean force obtained by atomistic simulations in aqueous solution. Following this approach, solvent mediation effects are included in the effective bead-bead nonbonded interactions and computationally very efficient (solvent-free) simulations of self-assembly processes can be performed. We show that the conformational properties of the all-atom dipeptide in explicit solvent can be accurately reproduced with the CG model. Moreover, preliminary simulations of peptide self-assembly performed with the CG model illustrate good agreement with results obtained from all-atom, explicit solvent simulations. PMID:19280018

  10. A solvent-free approach to extract the lipid fraction from sewer grease for biodiesel production.

    Science.gov (United States)

    Tu, Qingshi; Wang, Jingjing; Lu, Mingming; Brougham, Andrew; Lu, Ting

    2016-08-01

    Fats, oils and greases (FOG) are the number one cause of sewer pipe blockage and have been mostly disposed of as a waste until recently. This study investigated a low cost and environmentally friendly approach to extract the lipid fraction (fatty acids and glycerides for biodiesel production) from sewer grease (SG), i.e., FOGs obtained from wastewater treatment plants (WWTPs). The lipid fraction of the sewer grease was primarily in the form of free fatty acid (FFA), at 20.7wt%. An innovative solvent-free extraction approach was developed using waste cooking oil (WCO) to overcome the challenges of emulsion, impurities and high moisture content of the sewer grease. A 95% extraction yield of sewer grease was achieved under the optimum operating condition of 3.2:1 WCO-SG ratio (wt/wt), 70°C and 240min. In addition, the reusability of the WCO was also investigated. WCO can be used two to three times for sewer grease extraction with more than 90% extraction efficiency. PMID:27256783

  11. Eco-friendly all-carbon paper electronics fabricated by a solvent-free drawing method

    Science.gov (United States)

    Kanaparthi, Srinivasulu; Badhulika, Sushmee

    2016-03-01

    Here we report the fabrication of high-performance all-carbon temperature and infrared (IR) sensors with a solvent-free multiwalled carbon nanotube (MWCNT) trace as the sensing element and commercial graphite pencil trace as the electrical contact on recyclable and biodegradable cellulose filter paper without using any toxic materials or complex procedures. The temperature sensor shows a large negative temperature coefficient of resistance (TCR) in the range of -3100 ppm K-1 to -4900 ppm K-1, which is comparable to available commercial temperature sensors, and an activation energy of 34.85 meV. The IR sensor shows a high responsivity of 58.5 V W-1, which is greater than reported IR sensors with similar dimensions. A detailed study of the conduction mechanism in MWCNTs with temperature and the photo response with IR illumination was done and it was found that the conduction is due to thermally assisted hopping in band tails and the photo response is bolometric in nature. The successful fabrication of these sensors on cellulose filter paper with a comparable performance to existing components indicates that it is possible to fabricate high-performance electronics using low-cost, eco-friendly materials without the need for expensive clean-room processing techniques or harmful chemicals.

  12. Structural and Morphological Properties of Cr2O3 Nanoparticles Synthesized By Novel Solvent Free Method

    Directory of Open Access Journals (Sweden)

    Meenambika .R

    2014-02-01

    Full Text Available Nanoparticles of chromium oxide (Cr2O3 are widely used in many fields serving as catalysts, wear resistance materials, and advanced colorants. For the first time, we have reported the solvent free synthesis of Cr2O3 nanoparticles via microwave irradiation followed by calcinations at 200, 400, 600 and 800°C for 1h. The influence of calcination temperature on the particle size, microstructure and morphology was examined by X-ray diffraction, Scanning Electron Microscope (SEM and Transmission Electron Microscope (TEM, Elemental compositions have been estimated by energy dispersive X-ray Absorption EDAX and thermo gravimetrv analysis (TGA-DTA. The average particle size of the synthesized Cr2O3 nanoparticles is calculated using the Scherrer's formula and found to be of less than 60 nm and is compared with Williamson Hall method . It is found that the molar ratio 1:3 is considered to be the best proportion to synthesis Cr2O3nanoparticles. These results also indicate that there is an improvement in the crystallinity of Cr2O3 nanoparticles with the increase in the annealing temperature. As the process is simple and low-cost, it has the potential to be produced on a large scale.

  13. 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.

  14. In-Vitro Characterization and Oral Bioavailability of Organic Solvent-free Solid Dispersions Containing Telmisartan.

    Science.gov (United States)

    Cao, Yue; Shi, Li-Li; Cao, Qing-Ri; Yang, Mingshi; Cui, Jing-Hao

    2016-01-01

    Poorly water-soluble drugs often suffer from limited or irreproducible clinical response due to their low solubility and dissolution rate. In this study, organic solvent-free solid dispersions (OSF-SDs) containing telmisartan (TEL) were prepared using polyvinylpyrrolidone K30 (PVP K30) and polyethylene glycol 6000 (PEG 6000) as hydrophilic polymers, sodium hydroxide (NaOH) as an alkalizer, and poloxamer 188 as a surfactant by a lyophilization method. In-vitro dissolution rate and physicochemical properties of the OSF-SDs were characterized using the USP I basket method, differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and fourier transform-infrared (FT-IR) spectroscopy. In addition, the oral bioavailability of OSF-SDs in rats was evaluated by using TEL bulk powder as a reference. The dissolution rates of the OSF-SDs were significantly enhanced as compared to TEL bulk powder. The results from DSC, XRD showed that TEL was molecularly dispersed in the OSF-SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between TEL and its carriers. The OSF-SDs exhibited significantly higher AUC0-24 h and Cmax, but similar Tmax as compared to the reference. This study demonstrated that OSF-SDs can be a promising method to enhance the dissolution rate and oral bioavailability of TEL. PMID:27642309

  15. Production of Diacylglycerol-enriched Oil by Glycerolysis of Soybean Oil using a Bubble Column Reactor in a Solvent-free System.

    Science.gov (United States)

    Zhang, Ning; Yang, Xue; Fu, Junning; Chen, Qiong; Song, Ziliang; Wang, Yong

    2016-01-01

    In this study, diacylglycerol-enriched soybean oil (DESO) was synthesized through Lipozyme 435-catalyzed glycerolysis of soybean oil (SO) in a solvent-free system using a modified bubble column reactor. The effects of enzyme load, mole ratio of glycerol to soybean oil, reaction temperature, gas flow and reaction time on DAG production were investigated. The selected conditions were established as being enzyme load of 4 wt% (mass of substrates), glycerol/soybean oil mole ratio of 20:1, reaction temperature of 80°C, gas flow of 10.6 cm/min, and a reaction time of 2.5 h, obtaining the DAG content of 49.4±0.5 wt%. The reusability of Lipozyme 435 was evaluated by monitoring the contents of DAG, monoacylglycerol (MAG) and triacylglycerol (TAG) in 10 consecutive runs. After purified by one-step molecular distillation, the DAG content of 63.5±0.3 wt% was achieved in DESO. The mole ratio of 1, 3-DAG to 1, 2-DAG was 2:1 and the fatty acid composition had no significant difference from that of soybean oil. However, the thermal properties of DESO and SO had considerable differences. Polymorphic form of DESO were mainly the β form and minor amounts of the β' form. Granular aggregation and round-shaped crystals were detected in DESO. PMID:26876674

  16. Production of Diacylglycerol-enriched Oil by Glycerolysis of Soybean Oil using a Bubble Column Reactor in a Solvent-free System.

    Science.gov (United States)

    Zhang, Ning; Yang, Xue; Fu, Junning; Chen, Qiong; Song, Ziliang; Wang, Yong

    2016-01-01

    In this study, diacylglycerol-enriched soybean oil (DESO) was synthesized through Lipozyme 435-catalyzed glycerolysis of soybean oil (SO) in a solvent-free system using a modified bubble column reactor. The effects of enzyme load, mole ratio of glycerol to soybean oil, reaction temperature, gas flow and reaction time on DAG production were investigated. The selected conditions were established as being enzyme load of 4 wt% (mass of substrates), glycerol/soybean oil mole ratio of 20:1, reaction temperature of 80°C, gas flow of 10.6 cm/min, and a reaction time of 2.5 h, obtaining the DAG content of 49.4±0.5 wt%. The reusability of Lipozyme 435 was evaluated by monitoring the contents of DAG, monoacylglycerol (MAG) and triacylglycerol (TAG) in 10 consecutive runs. After purified by one-step molecular distillation, the DAG content of 63.5±0.3 wt% was achieved in DESO. The mole ratio of 1, 3-DAG to 1, 2-DAG was 2:1 and the fatty acid composition had no significant difference from that of soybean oil. However, the thermal properties of DESO and SO had considerable differences. Polymorphic form of DESO were mainly the β form and minor amounts of the β' form. Granular aggregation and round-shaped crystals were detected in DESO.

  17. 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.

  18. Reconstitution of Human Ion Channels into Solvent-free Lipid Bilayers Enhanced by Centrifugal Forces.

    Science.gov (United States)

    Hirano-Iwata, Ayumi; Ishinari, Yutaka; Yoshida, Miyu; Araki, Shun; Tadaki, Daisuke; Miyata, Ryusuke; Ishibashi, Kenichi; Yamamoto, Hideaki; Kimura, Yasuo; Niwano, Michio

    2016-05-24

    Artificially formed bilayer lipid membranes (BLMs) provide well-defined systems for functional analyses of various membrane proteins, including ion channels. However, difficulties associated with the integration of membrane proteins into BLMs limit the experimental efficiency and usefulness of such BLM reconstitution systems. Here, we report on the use of centrifugation to more efficiently reconstitute human ion channels in solvent-free BLMs. The method improves the probability of membrane fusion. Membrane vesicles containing the human ether-a-go-go-related gene (hERG) channel, the human cardiac sodium channel (Nav1.5), and the human GABAA receptor (GABAAR) channel were formed, and the functional reconstitution of the channels into BLMs via vesicle fusion was investigated. Ion channel currents were recorded in 67% of the BLMs that were centrifuged with membrane vesicles under appropriate centrifugal conditions (14-55 × g). The characteristic channel properties were retained for hERG, Nav1.5, and GABAAR channels after centrifugal incorporation into the BLMs. A comparison of the centrifugal force with reported values for the fusion force revealed that a centrifugal enhancement in vesicle fusion was attained, not by accelerating the fusion process but by accelerating the delivery of membrane vesicles to the surface of the BLMs, which led to an increase in the number of membrane vesicles that were available for fusion. Our method for enhancing the probability of vesicle fusion promises to dramatically increase the experimental efficiency of BLM reconstitution systems, leading to the realization of a BLM-based, high-throughput platform for functional assays of various membrane proteins.

  19. 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.

  20. A Novel One-Pot Green Synthesis of Dispirooxindolo-pyrrolidines via 1,3-Dipolar Cycloaddition Reactions of Azomethine Ylides

    Directory of Open Access Journals (Sweden)

    Abdulrahman I. Almansour

    2015-01-01

    Full Text Available A facile synthesis of dispirooxindolopyrrolidines has been accomplished via a one-pot three component 1,3-dipolar cycloaddition reaction. The reaction of azomethine ylides generated in situ from L-phenylalanine and substituted isatins with a series of unusual (E-2-oxoindolino-3-ylidene acetophenone dipolarophiles in the ionic liquid 1-butyl-3-methylimidazolium bromide [bmim]BF4, furnished the cycloadducts in good yields, with the regioisomers 5a–f being obtained with high selectivity. Furthermore, the recyclability of [bmim]BF4, up to five times, was also investigated.

  1. Pseudo five-component synthesis of 2,5-di(heteroarylthiophenes via a one-pot Sonogashira–Glaser cyclization sequence

    Directory of Open Access Journals (Sweden)

    Dominik Urselmann

    2011-11-01

    Full Text Available Based upon a consecutive one-pot Sonogashira–Glaser coupling–cyclization sequence a variety of 2,5-di(heteroarylthiophenes were synthesized in moderate to good yields. A single Pd/Cu-catalyst system, without further catalyst addition, and easily available, stable starting materials were used, resulting in a concise and highly efficient route for the synthesis of the title compounds. This novel pseudo five-component synthesis starting from iodo(heteroarenes is particularly suitable as a direct access to well-defined thiophene oligomers, which are of peculiar interest in materials science.

  2. T3P-Promoted, Mild, One-Pot Syntheses of Constrained Polycyclic Lactam Dipeptide Analogues via Stereoselective Pictet-Spengler and Meyers Lactamization Reactions.

    Science.gov (United States)

    Jida, Mouhamad; Van der Poorten, Olivier; Guillemyn, Karel; Urbanczyk-Lipkowska, Zofia; Tourwé, Dirk; Ballet, Steven

    2015-09-18

    A new convenient, mild, one-pot procedure is described for the diastereoselective synthesis of constrained 7,5- and 7,6-fused azabicycloalkanes. Using 2-formyl-L-tryptophan and 2-formyl-l-phenylalanine as bielectrophilic building blocks, T3P-mediated Pictet-Spengler and Meyers lactamization reactions were developed to present chiral and polycyclic aminoindolo- and aminobenzazepinone compounds in excellent yields. The conformationally constrained compounds can serve as templates for peptidomimetic research or polyheterocyclic privileged scaffolds. PMID:26322913

  3. One-pot synthesis of monodisperse palladium-copper nanocrystals supported on reduced graphene oxide nanosheets with improved catalytic activity and methanol tolerance for oxygen reduction reaction

    Science.gov (United States)

    Lv, Jing-Jing; Li, Shan-Shan; Wang, Ai-Jun; Mei, Li-Ping; Feng, Jiu-Ju; Chen, Jian-Rong; Chen, Zhaojiang

    2014-12-01

    Monodisperse bimetallic alloyed palladium-copper nanocrystals are uniformly supported on reduced graphene oxide nanosheets by a one-pot solvothermal strategy, with an average size of 6.81 nm. As a result, the as-prepared nanocomposites have the enlarged electrochemically active surface area (49.2 m2 g-1), and display the improved electrocatalytic performance and high methanol-tolerance ability for oxygen reduction reaction in alkaline media, compared with commercial Pd black and RGOs. Those RGOs-supporting Pd-Cu alloys would have potential applications in fuel cells.

  4. One-pot, three-component synthesis of highly substituted pyridines and 1,4-dihydropyridines by using nanocrystalline magnesium oxide

    Indian Academy of Sciences (India)

    M Lakshmi Kantam; Koosam Mahendar; Suresh Bhargava

    2010-01-01

    One pot, three component synthesis of 2-amino-4-aryl-3,5-dicyano-6-sulfanylpyridines and the corresponding 1,4-dihydropyridines are from readily accessible starting materials is described. Simply heating of an ethanolic solution of structurally diverse aldehydes with various thiols and malononitrile in the presence of nanocrystalline magnesium oxide provides the highly substituted pyridine derivatives in moderate to high yields, each representing a privileged medicinal scaffold with their structural motif. After completion of the reaction, the catalyst can be recovered efficiently and reused with constintent activity.

  5. One-pot synthesis of 4′-alkyl-4-cyanobiaryls on the basis of the terephthalonitrile dianion and neutral aromatic nitrile cross-coupling

    Science.gov (United States)

    Peshkov, Roman Yu; Chunyan, Wang; Tretyakov, Evgeny V; Shteingarts, Vitalij D

    2016-01-01

    Summary A convenient one-pot approach to alkylcyanobiaryls is described. The method is based on biaryl cross-coupling between the sodium salt of the terephthalonitrile dianion and a neutral aromatic nitrile in liquid ammonia, and successive alkylation of the long-lived anionic intermediate with alkyl bromides. The reaction is compatible with benzonitriles that contain methyl, methoxy and phenyl groups, fluorine atoms, and a 1-cyanonaphthalene residue. The variety of ω-substituted alkyl bromides, including an extra bromine atom, a double bond, cyano and ester groups, as well as a 1,3-dioxane fragment are suitable as alkylation reagents. PMID:27559409

  6. An efficient and scalable one-pot double Michael addition-Dieckmann condensation for the synthesis of 4,4-disubstituted cyclohexane beta-keto esters.

    Science.gov (United States)

    DeGraffenreid, Michael R; Bennett, Sarah; Caille, Sebastien; Gonzalez-Lopez de Turiso, Felix; Hungate, Randall W; Julian, Lisa D; Kaizerman, Jacob A; McMinn, Dustin L; Rew, Yosup; Sun, Daqing; Yan, Xuelei; Powers, Jay P

    2007-09-14

    A simple, scalable, and efficient one-pot methodology for the synthesis of 4,4-disubstituted cyclohexane beta-keto esters from benzylic nitriles or esters and methyl acrylate promoted by potassium tert-butoxide is described. The process relies on a tandem double Michael addition-Dieckmann condensation reaction, which results in the formation of three discrete carbon-carbon bonds in a single pot, including a quaternary center. The method allows for the convenient and rapid synthesis of a variety of 4-aryl-4-cyano-2-carbomethoxycyclohexanone and 4-aryl-2,4-biscarbomethoxycyclohexanone building blocks for use in natural products synthesis and medicinal chemistry. PMID:17696402

  7. One-pot synthesis of core-shell Cu@SiO2 nanospheres and their catalysis for hydrolytic dehydrogenation of ammonia borane and hydrazine borane

    OpenAIRE

    Qilu Yao; Zhang-Hui Lu; Zhujun Zhang; Xiangshu Chen; Yaqian Lan

    2014-01-01

    Ultrafine copper nanoparticles (Cu NPs) within porous silica nanospheres (Cu@SiO2) were prepared via a simple one-pot synthetic route in a reverse micelle system and characterized by SEM, TEM, EDX, XRD, N2 adsorption-desorption, CO-TPD, XPS, and ICP methods. The characterized results show that ultrafine Cu NPs with diameter of around 2 nm are effectively embedded in the center of well-proportioned spherical SiO2 NPs of about 25 nm in diameter. Compared to commercial SiO2 supported Cu NPs, SiO...

  8. Facile synthesis of 1H-imidazo[1,2-b]pyrazoles via a sequential one-pot synthetic approach

    Directory of Open Access Journals (Sweden)

    András Demjén

    2014-10-01

    Full Text Available 5-Aminopyrazole-4-carbonitrile and ethyl 5-aminopyrazole-4-carboxylate, as potential trifunctional building blocks are introduced in a facile, chemo- and regioselective multicomponent assembly of imidazo[1,2-b]pyrazoles via the Groebke–Blackburn–Bienaymé reaction (GBB reaction. Besides the synthetic elaboration of a green-compatible isocyanide-based access in three-component mode, we describe an operationally simple, one-pot two-step GBB protocol for the rapid construction of a 46 membered imidazo[1,2-b]pyrazole library with yields up to 83%.

  9. One-pot green synthesis of 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives as a new class of tyrosinase inhibitors.

    Science.gov (United States)

    Zheng, Zong-Ping; Zhang, Yi-Nan; Zhang, Shuang; Chen, Jie

    2016-02-01

    A new method was developed for one-pot green synthesis 1,3,5-triarylpentane-1,5-dione, triarylmethane, and flavonoid derivatives from the reaction between 2,4-dihydroxybenzaldehyde and hydroxyacetophenones via Aldol, Michael, and Friedel-Crafts additions using boric acid as catalyst in polyethylene glycol 400. The synthetic compounds demonstrated significant tyrosinase inhibitory activities much stronger than that of kojic acid. More important, 1,3,5-triarylpentane-1,5-dione and triarylmethane derivatives were found to be a new class of tyrosinase inhibitors.

  10. Nano-TiCl4/SiO2: An efficient heterogeneous solid acid catalyst for the one pot cascade five-component synthesis of densely functionalized tetrahydropyridines

    Indian Academy of Sciences (India)

    Abdolhamid Bamoniri; Bi Bi Fatemeh Mirjalili; Reza Tarazian

    2015-05-01

    Nano-TiCl4/SiO2 was found to be an inexpensive and efficient heterogeneous solid acid catalyst for the synthesis of one-pot cascade synthesis of highly functionalized asymmetric tetrahydropyridines from the five-component condensation reaction of the para-substituted anilines and aromatic aldehydes with ethyl acetoacetate under thermal conditions. Novel methodology, environmentally benign conditions, clean protocol, easy work-up and high yields are the important advantages of this protocol. The products were characterized using physical and spectroscopic data such as FT-IR, 1H-NMR and in some cases 13C-NMR and CHN analysis.

  11. Multicomponent versus domino reactions: One-pot free-radical synthesis of β-amino-ethers and β-amino-alcohols

    Directory of Open Access Journals (Sweden)

    Bianca Rossi

    2015-01-01

    Full Text Available Following an optimized multicomponent procedure, an aryl amine, a ketone, and a cyclic ether or an alcohol molecule are assembled in a one-pot synthesis by nucleophilic radical addition of ketyl radicals to ketimines generated in situ. The reaction occurs under mild conditions by mediation of the TiCl4/Zn/t-BuOOH system, leading to the formation of quaternary β-amino-ethers and -alcohols. The new reaction conditions guarantee good selectivity by preventing the formation of secondary products. The secondary products are possibly derived from a competitive domino reaction, which involves further oxidation of the ketyl radicals.

  12. A Convenient One-pot Preparation of Acetorhamnose-sidases Compounds%一锅法制备乙酰溴代鼠李糖

    Institute of Scientific and Technical Information of China (English)

    苗长庆

    2011-01-01

    Acetorhamnose-sidases was synthesized directly from one-pot reaction of rhamnose,Ac2O and HBr/HOAc.This preparation of acetorhamnose-sidases is convenient in operation and has high yield.%将鼠里糖与醋酸酐及溴化氢的冰醋酸溶液一锅反应直接得到三乙酰溴代鼠里糖.这种方法制备三乙酰溴代鼠里糖操作方便,收率高.

  13. One-pot synthesis of pyrido[2,3-d]pyrimidine derivatives using sulfonic acid functionalized SBA-15 and the study on their antimicrobial activities

    Directory of Open Access Journals (Sweden)

    Ghodsi Mohammadi Ziarani

    2015-11-01

    Full Text Available A simple and clean one-pot method for the preparation of 7-amino-2,4-dioxo-5-aryl-1,2,3,4-tetrahydropyrido[2,3-d]pyrimidine-6-carbonitrile derivatives using 6-amino uracil, various aromatic aldehydes and malononitrile in the presence of sulfonic acid functionalized SBA-15 (SBA-Pr-SO3H is described. Some of synthesized pyrido[2,3-d]pyrimidines showed antimicrobial activities against some fungi and gram positive and negative bacteria.

  14. 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.

  15. Fe-Al/clay as an efficient heterogeneous catalyst for solvent-free synthesis of 3, 4-dihydropyrimidones

    Indian Academy of Sciences (India)

    Bashir A Dar; Praveen Patidar; Sunil Kumar; Mohammad Arif Wagay; Akshay K Sahoo; Parduman R Sharma; Sanjay Pandey; Meena Sharma; Baldev Singh

    2013-05-01

    A practical, efficient, environmentally benign condensation of an aldehyde, ethylacetoacetate and urea/thiourea for the synthesis of 3, 4-dihydropyrimidinones, employing Fe-Al/clay composite catalyst is described. The process has been carried out under solvent-free conditions in the presence of very small amount of catalyst. The catalyst used for this process is easy to prepare, easy to handle, cost effective, easy to separate and recyclable at least up to 5 cycles with good to excellent yield.

  16. Preparation of Silyl Ethers Using Hexamethyldisilazane in the Presence of N-Bromosuccinimide under Mild and Solvent-Free Conditions

    Institute of Scientific and Technical Information of China (English)

    SHATERIAN Hamid Reza; DOOSTMOHAMMADI Razieh; GHASHANG Majid

    2008-01-01

    A mild,simple,novel and highly efficient method for the rapid protection of various primary,secondary,tertiary aliphatic and aromatic alcohols using hexamethyldisilazane (HMDS) in the presence of N-bromosuccinimide (NBS) as an active,inexpensive,non-toxic and readily available catalyst under solvent-free conditions is described.Trimethylsilyl ethers were prepared in high to excellent yields with short reaction time under mild and almost neutral reaction conditions.

  17. Application of 2k Full Factorial Design in Optimization of Solvent-Free Microwave Extraction of Ginger Essential Oil

    OpenAIRE

    Mumtaj Shah; 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 ...

  18. Solvent-free phase-vanishing reactions with PTFE (Teflon®) as a phase screen

    OpenAIRE

    Kevin Pels; Veljko Dragojlovic

    2009-01-01

    In a solvent-free phase-vanishing reaction with PTFE (polytetrafluoroethylene, Teflon®) tape as the phase screen, a thermometer adapter is utilized to insert a PTFE-sealed tube into the vapor phase above the substrate. Besides avoiding use of solvents, the experimental design is not dependent upon the densities of the reactants and the procedure generates little or no waste while providing the reaction products in high yield and in high purity.

  19. TMSCl-catalysed condensation of -diketone compounds with urea/thiourea derivatives under solvent-free conditions

    Indian Academy of Sciences (India)

    Akbar Mobinikhaledi; Alireza Khajeh Amiri

    2013-09-01

    An efficient, rapid and green synthesis of glycoluril, imidazolidine-2-one, imidazole-2-one and imidazole-2-thiol derivatives have been accomplished by the reaction of urea/thiourea derivatives and -diketone at 100°C in the presence of trimethylsilyl chloride (TMSCl) as Lewis acid catalyst under solvent-free conditions. This approach offers many advantages such as good product yields, various products, short reaction time, easy isolation of products, facile purification and environmentally benign reaction conditions.

  20. 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.