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Sample records for highly diastereoselective synthesis

  1. Highly Diastereoselective Synthesis of 2-(1-N-Boc-aminoalkyl)thiazole-5-carboxylates by Reduction of tert-Butylsulfinyl Ketimines.

    Science.gov (United States)

    Magata, Takuji; Hirokawa, Yoshimi; Furokawa, Aya; Takeuchi, Kazuhisa; Ohtomo, Yoshiaki; Kino, Toshitaka; Kominami, Jun; Nakai, Yuto; Kitamura, Maria; Maezaki, Naoyoshi

    2018-01-01

    Positional isomers of naturally occurring peptide subunits were synthesized via highly diastereoselective reduction of tert-butylsulfinyl ketimines as a key reaction. While NaBH 4 reduction of ketimines derived from 2-thiazolyl ketones afforded the (R S ,R)-isomer with moderate diastereoselectivity, L-Selectride ® reduction afforded the (R S ,S)-isomer as the sole product. In contrast, ketimines derived from tert-butyl 2-thiazolyl ketone afforded the (R S ,R)-isomer with low diastereoselectivity by both NaBH 4 and L-Selectride ® reduction. Stereochemistry of the reaction was discussed based on calculation of the conformational energies for ketimines.

  2. Tandem Oxidative Derivatization of Nitrene Insertion Products for the Highly Diastereoselective Synthesis of 1,3-aminoalcohols.

    Science.gov (United States)

    Alderson, Juliet M; Schomaker, Jennifer M

    2017-06-27

    Transition-metal-catalyzed nitrene insertion into tertiary C-H bonds located at stereogenic carbons often results in mixtures of diastereomeric products, especially if the reaction proceeds through a concerted pathway. In this communication, we report a solution to this problem that invokes a one-pot, silver-catalyzed C-H nitrene transfer reaction. Nitrene insertion is followed by facile oxidation of the amine to an imine and nucleophilic addition to furnish α-tertiary amine 1,3-aminoalcohol products in high diastereoselectivities. The silver catalyst, PhIO oxidant, and TEMPO additive are crucial to success in this unusual oxidation, which is proposed to occur via hydrogen-atom abstraction from pre-activation of the initial nitrene insertion product by additional oxidant. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Facile and Highly Diastereoselective Synthesis of syn- and cis-1,2-Diol Derivatives from Protected alpha-Hydroxy Ketones

    Czech Academy of Sciences Publication Activity Database

    Jahn, Emanuela; Smrček, Jakub; Pohl, Radek; Císařová, I.; Jones, P. G.; Jahn, Ullrich

    2015-01-01

    Roč. 2015, č. 35 (2015), s. 7785-7798 ISSN 1434-193X Grant - others:COST(XE) CM1201 Institutional support: RVO:61388963 Keywords : synthetic methods * reduction * diastereoselectivity * diols * ketones Subject RIV: CC - Organic Chemistry Impact factor: 3.068, year: 2015

  4. Diastereoselective multicomponent synthesis of dihydropyridones with an isocyanide functionality

    NARCIS (Netherlands)

    Paravidino, M.; Bon, R.S.; Scheffelaar, R.; Vugts, D.J.; Znabet, A.; Schmitz, R.F.; de Kanter, F.J.J.; Lutz, M.; Spek, A.L; Groen, M.B.; Orru, R.V.A.

    2006-01-01

    In a search for new multicomponent strategies leading to valuable small heterocycles, a new highly diastereoselective four-component reaction (4CR) was found in which a phosphonate, nitriles, aldehydes, and isocyanoacetates combine to afford functionalized 3-isocyano-3,4-dihydro-2-pyridones. In this

  5. Diastereoselective synthesis of tetrahydropyrans via Prins-Ritter and Prins-arylthiolation cyclization reactions.

    Science.gov (United States)

    Hazarika, Nabajyoti; Sarmah, Barnali; Bordoloi, Manobjyoti; Phukan, Prodeep; Baishya, Gakul

    2017-03-01

    An efficient method has been developed for the synthesis of two new classes of tetrahydropyran derivatives comprising amide, tetrazole or benzothiazole moieties via a three-component reaction of 6-methylhept-5-en-2-ol, arylaldehydes and nitriles/thiols in the presence of a tetrafluoroboric acid diethyl ether complex. The reaction proceeds via the formation of an oxocarbenium ion. This protocol is highly diastereoselective and only single diastereomer has been isolated in each case.

  6. Highly Diastereoselective Indium-Mediated Allylation of Proline-Derived Hydrazones

    International Nuclear Information System (INIS)

    Satyender, Apuri; Jang, Doo Ok

    2013-01-01

    A highly diastereoselective indium-mediated addition reaction to L-proline-derived hydrazones has been developed. The method affords an efficient and general synthesis of homoallylic amines of high optically purity in high yields and diastereomeric ratios up to 98:2. It is well known that (S)-1-amino-2-methoxymethylpyrro-lidine and (S)-4-isopropyl- or (S)-4-phenylmethyl-oxa-zolidin-2-one-derived hydrazones have been used for metal-mediated diastereoselective allylation additions to produce chiral homoallylic amines. However, the optically pure hydrazine precursors are either commercially expensive and/or involve laborious synthetic procedures employing toxic reagents for their preparation. Thus, the design of novel classes of chiral hydrazines that would further broaden the scope of asymmetric synthesis to access optically pure homoallylic amines is highly desirable

  7. Diastereoselective synthesis of trans-2,3-dihydrofuro[3,2-c]coumarins by MgO nanoparticles under ultrasonic irradiation

    Directory of Open Access Journals (Sweden)

    Javad Safaei-Ghomi

    2017-12-01

    Full Text Available MgO nanoparticles have been used as an efficient catalyst for the diastereoselective preparation of trans-2-benzoyl-3-(aryl-2H-furo[3,2-c]chromen-4(3H-ones by the multi-component reaction of 2,4′-dibromoacetophenone, pyridine, benzaldehydes and 4-hydroxycoumarin under ultrasonic irradiation. This interesting result revealed that the pyridiniumylide assisted tandem three-component coupling reaction is highly diastereoselective. Atom economy, wide range of products, high catalytic activity, excellent yields in short reaction times, diastereoselective synthesis and environmental benignity are some of the important features of this protocol. Keywords: Furo[3,2-c]coumarins, Ultrasonic irradiation, MgO nanoparticles, Diastereoselective, One-pot syntheses

  8. Highly efficient and diastereoselective gold(I)-catalyzed synthesis of tertiary amines from secondary amines and alkynes: substrate scope and mechanistic insights.

    Science.gov (United States)

    Liu, Xin-Yuan; Guo, Zhen; Dong, Sijia S; Li, Xiao-Hua; Che, Chi-Ming

    2011-11-11

    An efficient method for the synthesis of tertiary amines through a gold(I)-catalyzed tandem reaction of alkynes with secondary amines has been developed. In the presence of ethyl Hantzsch ester and [{(tBu)(2)(o-biphenyl)P}AuCl]/AgBF(4) (2 mol %), a variety of secondary amines bearing electron-deficient and electron-rich substituents and a wide range of alkynes, including terminal and internal aryl alkynes, aliphatic alkynes, and electron-deficient alkynes, underwent a tandem reaction to afford the corresponding tertiary amines in up to 99 % yield. For indolines bearing a preexisting chiral center, their reactions with alkynes in the presence of ethyl Hantzsch ester catalyzed by [{(tBu)(2)(o-biphenyl)P}AuCl]/AgBF(4) (2 mol %) afforded tertiary amines in excellent yields and with good to excellent diastereoselectivity. All of these organic transformations can be conducted as a one-pot reaction from simple and readily available starting materials without the need of isolation of air/moisture-sensitive enamine intermediates, and under mild reaction conditions (mostly room temperature and mild reducing agents). Mechanistic studies by NMR spectroscopy, ESI-MS, isotope labeling studies, and DFT calculations on this gold(I)-catalyzed tandem reaction reveal that the first step involving a monomeric cationic gold(I)-alkyne intermediate is more likely than a gold(I)-amine intermediate, a three-coordinate gold(I) intermediate, or a dinuclear gold(I)-alkyne intermediate. These studies also support the proposed reaction pathway, which involves a gold(I)-coordinated enamine complex as a key intermediate for the subsequent transfer hydrogenation with a hydride source, and reveal the intrinsic stereospecific nature of these transformations observed in the experiments. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Synthetic Progress toward Azadirachtins. 1. Enantio- and Diastereoselective Synthesis of the Left-Wing Fragment of 11-epi-Azadirachtin I.

    Science.gov (United States)

    Shi, Hang; Tan, Ceheng; Zhang, Weibin; Zhang, Zichun; Long, Rong; Luo, Tuoping; Yang, Zhen

    2015-05-15

    A highly enantio- and diastereoselective synthesis of the left-wing fragment of 11-epi-azadirachtin I characterized with the pairwise use of palladium- and gold-catalyzed cascade reactions is presented. By enlisting a sequence of stereocontrolled transformations, our 21-step route established the stereocenters of the left-wing fragment from one chiral starting material, (-)-carvone, which would significantly facilitate the synthetic studies of the azadirachtin-type limonoids.

  10. Combining cycloisomerization with trienamine catalysis: a regiochemically flexible enantio- and diastereoselective synthesis of hexahydroindoles.

    Science.gov (United States)

    Chintalapudi, V; Galvin, E A; Greenaway, R L; Anderson, E A

    2016-01-14

    The synthesis of polysubstituted hexahydroindoles through trienamine-organocatalyzed cycloadditions of pyrrolidinyl dienals, prepared by palladium-catalyzed cycloisomerization, is reported. The cycloadditions of this novel class of dienals proceed with excellent levels of enantio- and diastereoselectivity, with the regioselectivity of cycloaddition with respect to the tethering ring readily tuned through design of the cycloisomerization substrate. This work culminates in the first examples of double-stereodifferentiating trienamine catalysis, where catalyst stereocontrol dominates facial selectivity in the cycloaddition, affording azacyclic products that are specifically functionalized at every position.

  11. Synthesis of Substituted Oxo-Azepines by Regio- and Diastereoselective Hydroxylation

    Directory of Open Access Journals (Sweden)

    Harold Spedding

    2017-10-01

    Full Text Available Substituted seven-membered N-heterocycles are prevalent bioactive epitopes and useful synthons for preparing enzyme inhibitors or molecular recognition systems. To fully exploit the chemical properties of this flexible N-heterocycle scaffold, efficient methods for its diverse functionalization are required. Here we utilize the late-stage oxidation of tetrahydroazepines as an approach to access densely functionalized oxo-azepines in a total of 8 steps and ~30% overall yield from commercially available starting materials. Hydroboration of tetrahydroazepines proceeded with diastereoselectivity in a substrate-dependent manner to yield regioisomeric azepanols before their oxidation to the corresponding oxo-azepines. Regioselectivity of the hydroboration step may be improved moderately by a rhodium catalyst, albeit with loss of conversion to a competing hydrogenation pathway. Overall our method allows efficient access to azepanols and oxo-azepines as versatile epitopes and synthons with a high degree of diastereoselectivity and moderate regioselectivity.

  12. Acylation, Diastereoselective Alkylation, and Cleavage of an Oxazolidinone Chiral Auxiliary: A Multistep Asymmetric Synthesis Experiment for Advanced Undergraduates

    Science.gov (United States)

    Smith, Thomas E.; Richardson, David P.; Truran, George A.; Belecki, Katherine; Onishi, Megumi

    2008-01-01

    An introduction to the concepts and experimental techniques of diastereoselective synthesis using a chiral auxiliary is described. The 4-benzyl-2-oxazolidinone chiral auxiliary developed by Evans is acylated with propionic anhydride under mild conditions using DMAP as an acyl transfer catalyst. Deprotonation with NaN(TMS)[subscript 2] at -78…

  13. Sequential Multicomponent Strategy for the Diastereoselective Synthesis of Densely Functionalized Spirooxindole-Fused Thiazolidines.

    Science.gov (United States)

    Rainoldi, Giulia; Begnini, Fabio; de Munnik, Mariska; Lo Presti, Leonardo; Vande Velde, Christophe M L; Orru, Romano; Lesma, Giordano; Ruijter, Eelco; Silvani, Alessandra

    2018-02-12

    We developed two Ugi-type three-component reactions of spirooxindole-fused 3-thiazolines, isocyanides, and either carboxylic acids or trimethylsilyl azide, to give highly functionalized spirooxindole-fused thiazolidines. Two diverse libraries were generated using practical and robust procedures affording the products in typically good yields. The obtained thiazolidines proved to be suitable substrates for further transformations. Notably, both the Ugi-Joullié and the azido-Ugi reactions resulted highly diastereoselective, affording predominantly the trans-configured products, as confirmed by X-ray crystallographic analysis.

  14. Thermally Stable Dialkylzirconocenes with β-Hydrogens. Synthesis and Diastereoselectivity

    OpenAIRE

    Wendt, Ola F.; Bercaw, John E.

    2001-01-01

    Alkylation of Cp^r_2ZrCl_2 (Cpr = Cp (η^5-C_5H_5), Cp‘ (η^5-C_5H_4Me), Cp^* (η^5-C_5Me_5)) and CpCp^*Zr(CH_3)Cl with 1-lithio-2-methylpentane (R^1Li) gives the corresponding dialkylzirconocenes Cp^r_2ZrR^1_2 and CpCp^*Zr(CH_3)R^1, in high yields. Such alkyls have unprecedented thermal stabilities, especially for the CpCp^* ligand framework. The diastereomers of the Cp^r_2ZrR^1_2 complexes are formed in a statistical distribution, whereas the diastereomers of CpCp^*Zr(CH_3)R^1 form in a 2:3 ra...

  15. Synthetic Progress toward Azadirachtins. 2. Enantio- and Diastereoselective Synthesis of the Right-Wing Fragment of 11-epi-Azadirachtin I.

    Science.gov (United States)

    Tan, Ceheng; Chen, Wei; Mu, Xinpeng; Chen, Qi; Gong, Jianxian; Luo, Tuoping; Yang, Zhen

    2015-05-15

    A stereoselective three-component coupling reaction of allylzinc bromide, silyl glyoxylate, and a β-lactone has been developed. This has been successfully applied to the enantio- and diastereoselective synthesis of the fully functionalized furopyran moiety of azadirachtins.

  16. Post-Ugi gold-catalyzed diastereoselective domino cyclization for the synthesis of diversely substituted spiroindolines

    Directory of Open Access Journals (Sweden)

    Amit Kumar

    2013-10-01

    Full Text Available An Ugi four-component reaction of propargylamine with 3-formylindole and various acids and isonitriles produces adducts which are subjected to a cationic gold-catalyzed diastereoselective domino cyclization to furnish diversely substituted spiroindolines. All the reactions run via an exo-dig attack in the hydroarylation step followed by an intramolecular diastereoselective trapping of the imminium ion. The whole sequence is atom economic and the application of a multicomponent reaction assures diversity.

  17. A General and Simple Diastereoselective Reduction by L-Selectride: Efficient Synthesis of Protected (4S,5S)-Dihydroxy Amides

    OpenAIRE

    Yin; Ye; Yu; Liu

    2010-01-01

    A general approach to (4S,5S)-4-benzyloxy-5-hydroxy-N-(4-methoxybenzyl) amides 10 based on a diastereoselective reduction of (5S,6RS)-6-alkyl-5-benzyloxy-6-hydroxy-2-piperidinones 6 and their tautomeric ring-opened keto amides 7 is described. The reduction with L-Selectride at -20 °C to room temperature afforded the products 10 in excellent yields and moderate to high syn-diastereoselectivities.

  18. A General and Simple Diastereoselective Reduction by L-Selectride: Efficient Synthesis of Protected (4S,5S-Dihydroxy Amides

    Directory of Open Access Journals (Sweden)

    Bo Yin

    2010-04-01

    Full Text Available A general approach to (4S,5S-4-benzyloxy-5-hydroxy-N-(4-methoxybenzyl amides 10 based on a diastereoselective reduction of (5S,6RS-6-alkyl-5-benzyloxy-6-hydroxy-2-piperidinones 6 and their tautomeric ring-opened keto amides 7 is described. The reduction with L-Selectride at -20 °C to room temperature afforded the products 10 in excellent yields and moderate to high syn-diastereoselectivities.

  19. A general and simple diastereoselective reduction by L-Selectride: efficient synthesis of protected (4S,5S)-dihydroxy amides.

    Science.gov (United States)

    Yin, Bo; Ye, Dong-Nai; Yu, Kai-Hui; Liu, Liang-Xian

    2010-04-16

    A general approach to (4S,5S)-4-benzyloxy-5-hydroxy-N-(4-methoxybenzyl) amides 10 based on a diastereoselective reduction of (5S,6RS)-6-alkyl-5-benzyloxy-6-hydroxy-2-piperidinones 6 and their tautomeric ring-opened keto amides 7 is described. The reduction with L-Selectride at -20 degrees C to room temperature afforded the products 10 in excellent yields and moderate to high syn-diastereoselectivities.

  20. Graphene oxide as a catalyst for the diastereoselective transfer hydrogenation in the synthesis of prostaglandin derivatives.

    Science.gov (United States)

    Coman, Simona M; Podolean, Iunia; Tudorache, Madalina; Cojocaru, Bogdan; Parvulescu, Vasile I; Puche, Marta; Garcia, Hermenegildo

    2017-09-14

    Modification of GO by organic molecules changes its catalytic activity in the hydrogen transfer from i-propanol to enones, affecting the selectivity to allyl alcohol and diastereoselectivity to the resulting stereoisomers. It is noteworthy the system does not contain metals and is recyclable.

  1. Diastereoselective Au-Catalyzed Allene Cycloisomerizations to Highly Substituted Cyclopentenes.

    Science.gov (United States)

    Reeves, Ryan D; Phelps, Alicia M; Raimbach, William A T; Schomaker, Jennifer M

    2017-07-07

    Site- and regiocontrolled Au-catalyzed allene carbocyclizations furnish highly substituted cyclopentenes in >1:1 dr. Significant substitution on the substrate is tolerated, with potential to install five contiguous stereocenters after alkene functionalization. Major challenges include identifying a Au/Cu catalyst that controls both the relative rates of allene epimerization/cyclization and the facial selectivity in addition of a metal enolate to the allene. Experiments to achieve stereodivergent cyclizations and transform key cyclopentenes into useful synthetic building blocks are described.

  2. Diastereoselective synthesis of trans-2,3-dihydrofuro[3,2-c]coumarins by MgO nanoparticles under ultrasonic irradiation

    OpenAIRE

    Javad Safaei-Ghomi; Pouria Babaei; Hossein Shahbazi-Alavi; Safura Zahedi

    2017-01-01

    MgO nanoparticles have been used as an efficient catalyst for the diastereoselective preparation of trans-2-benzoyl-3-(aryl)-2H-furo[3,2-c]chromen-4(3H)-ones by the multi-component reaction of 2,4â²-dibromoacetophenone, pyridine, benzaldehydes and 4-hydroxycoumarin under ultrasonic irradiation. This interesting result revealed that the pyridiniumylide assisted tandem three-component coupling reaction is highly diastereoselective. Atom economy, wide range of products, high catalytic activity, ...

  3. A Microwave-Assisted Diastereoselective Multicomponent Reaction To Access Dibenzo[c,e]azepinones: Synthesis and Biological Evaluation

    NARCIS (Netherlands)

    Mehta, V.P.; Modha, S.G.; Ruijter, E.; van Hecke, K.; van Meervelt, L.; Pannecouque, C.; Balzarini, J.; Orru, R.V.A.; van der Eycken, E.

    2011-01-01

    An unprecedented microwave-assisted multicomponent strategy has been elaborated for the fast, efficient, and diastereoselective generation of the dibenzo[c,e]azepinone scaffold. The generated compounds were evaluated for their bioactivity. © 2011 American Chemical Society.

  4. Stereoselective synthesis of the Halaven C14-C26 fragment from D-quinic acid: crystallization-induced diastereoselective transformation of an α-methyl nitrile.

    Science.gov (United States)

    Belanger, Francis; Chase, Charles E; Endo, Atsushi; Fang, Francis G; Li, Jing; Mathieu, Steven R; Wilcoxen, Annie Z; Zhang, Huiming

    2015-04-20

    Crystallization-induced diastereoselective transformation (CIDT) of an α-methyl nitrile completes an entirely non-chromatographic synthesis of the halichondrin B C14-C26 stereochemical array. The requisite α-methyl nitrile substrate is derived from D-quinic acid through a series of substrate-controlled stereoselective reactions via a number of crystalline intermediates that benefit from a rigid polycyclic template. Therefore, all four stereogenic centers in the Halaven C14-C26 fragment were derived from the single chiral source D-quinic acid. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Nonradical Zinc-Barbier Reaction for Diastereoselective Synthesis of Vicinal Amino Alcohols

    DEFF Research Database (Denmark)

    Keinicke, Lise Edelmann; Fristrup, Peter; Norrby, Per-Ola

    2005-01-01

    A new protocol for the synthesis of vicinal amino alcohols is described. The method employs a Barbier-type reaction between an imine and 3-benzoyloxyallyl bromide in the presence of zinc metal. The addition products are debenzoylated to afford amino alcohols in good yields and with diastereomeric...

  6. IBX-mediated oxidation of unactivated cyclic amines: application in highly diastereoselective oxidative Ugi-type and aza-Friedel-Crafts reactions.

    Science.gov (United States)

    de Graaff, C; Bensch, L; van Lint, Matthijs J; Ruijter, E; Orru, R V A

    2015-10-28

    The first o-iodoxybenzoic acid (IBX) mediated oxidation of unactivated amines to imines is described. A range of meso-pyrrolidines were shown to be suitable substrates. The chemical space was further explored with one-pot oxidative Ugi-type and aza-Friedel-Crafts reactions, which proved to be highly diastereoselective.

  7. Sequential Multicomponent Strategy for the Diastereoselective Synthesis of Densely Functionalized Spirooxindole-Fused Thiazolidines

    NARCIS (Netherlands)

    Rainoldi, Giulia; Begnini, Fabio; De Munnik, Mariska; Lo Presti, Leonardo; Vande Velde, Christophe M.L.; Orru, Romano; Lesma, Giordano; Ruijter, Eelco; Silvani, Alessandra

    2018-01-01

    We developed two Ugi-type three-component reactions of spirooxindole-fused 3-thiazolines, isocyanides, and either carboxylic acids or trimethylsilyl azide, to give highly functionalized spirooxindole-fused thiazolidines. Two diverse libraries were generated using practical and robust procedures

  8. Diastereoselective Synthesis of the Aminocyclitol Core of Jogyamycin via an Allene Aziridination Strategy.

    Science.gov (United States)

    Gerstner, Nels C; Adams, Christopher S; Grigg, R David; Tretbar, Maik; Rigoli, Jared W; Schomaker, Jennifer M

    2016-01-15

    Oxidative allene amination provides rapid access to densely functionalized amine-containing stereotriads through highly reactive bicyclic methyleneaziridine intermediates. This strategy has been demonstrated as a viable approach for the construction of the densely functionalized aminocyclitol core of jogyamycin, a natural product with potent antiprotozoal activity. Importantly, the flexibility of oxidative allene amination will enable the syntheses of modified aminocyclitol analogues of the jogyamycin core.

  9. L-Selectride-Mediated Highly Diastereoselective Asymmetric Reductive Aldol Reaction: Access to an Important Subunit for Bioactive Molecules

    OpenAIRE

    Ghosh, Arun K.; Kass, Jorden; Anderson, David D.; Xu, Xiaoming; Marian, Christine

    2008-01-01

    L-Selectride reduction of a chiral or achiral enone followed by reaction of the resulting enolate with optically active α-alkoxy aldehydes proceeded with excellent diastereoselectivity. The resulting α,α-dimethyl-β-hydroxy ketones are inherent to a variety of biologically active natural products.

  10. L-selectride-mediated highly diastereoselective asymmetric reductive aldol reaction: access to an important subunit for bioactive molecules.

    Science.gov (United States)

    Ghosh, Arun K; Kass, Jorden; Anderson, David D; Xu, Xiaoming; Marian, Christine

    2008-11-06

    L-selectride reduction of a chiral or achiral enone followed by reaction of the resulting enolate with optically active alpha-alkoxy aldehydes proceeded with excellent diastereoselectivity. The resulting alpha,alpha-dimethyl-beta-hydroxy ketones are inherent to a variety of biologically active natural products.

  11. Diastereoselective and enantioselective reduction of tetralin-1,4-dione

    Directory of Open Access Journals (Sweden)

    2008-10-01

    Full Text Available BackgroundThe chemistry of tetralin-1,4-dione, the stable tautomer of 1,4-dihydroxynaphthalene, has not been explored previously. It is readily accessible and offers interesting opportunities for synthesis.ResultsThe title reactions were explored. L-Selectride reduced the diketone to give preferentially the cis-diol (d.r. 84 : 16. Red-Al gave preferentially the trans-diol (d.r. 13 : 87. NaBH4, LiAlH4, and BH3 gave lower diastereoselectivities (yields: 76–98%. Fractional crystallization allowed isolation of the cis-diol and the trans-diol (55% and 66% yield, respectively. Borane was used to cleanly give the mono-reduction product. Highly enantioselective CBS reductions afforded the trans-diol (72% yield, 99% ee and the mono-reduction product (81%, 95% ee.ConclusionDiastereoselective and enantioselective reductions of the unexplored tetralin-1,4-dione provides a very convenient entry into a number of synthetically highly attractive 1,4-tetralindiols and 4-hydroxy-1-tetralone.

  12. Diastereoselective and enantioselective reduction of tetralin-1,4-dione.

    Science.gov (United States)

    Kündig, E Peter; Enriquez-Garcia, Alvaro

    2008-01-01

    The chemistry of tetralin-1,4-dione, the stable tautomer of 1,4-dihydroxynaphthalene, has not been explored previously. It is readily accessible and offers interesting opportunities for synthesis. The title reactions were explored. L-Selectride reduced the diketone to give preferentially the cis-diol (d.r. 84 : 16). Red-Al gave preferentially the trans-diol (d.r. 13 : 87). NaBH(4), LiAlH(4), and BH(3) gave lower diastereoselectivities (yields: 76-98%). Fractional crystallization allowed isolation of the cis-diol and the trans-diol (55% and 66% yield, respectively). Borane was used to cleanly give the mono-reduction product. Highly enantioselective CBS reductions afforded the trans-diol (72% yield, 99% ee) and the mono-reduction product (81%, 95% ee). Diastereoselective and enantioselective reductions of the unexplored tetralin-1,4-dione provides a very convenient entry into a number of synthetically highly attractive 1,4-tetralindiols and 4-hydroxy-1-tetralone.

  13. Diastereoselective Synthesis of 5-Hydroxy-8-methoxy-1-oxaspiro[5,5]undeca-7,10-diene-9-one

    Directory of Open Access Journals (Sweden)

    Thomas W. Scully

    2013-01-01

    Full Text Available A short five steps synthesis of the title compound from vanillin is described. The racemic spiroether 7 was obtained in 61% yield and in >99% diastereomeric excess (by 1H-NMR from the corresponding phenolic derivative 3 by oxidation with lead (IV acetate.

  14. Aldolase catalyzed L-phenylserine synthesis in a slug-flow microfluidic system - Performance and diastereoselectivity studies

    NARCIS (Netherlands)

    Čech, J.; Hessel, V.; Přibyl, M.

    2017-01-01

    We study synthesis of . L-phenylserine catalyzed by the enzyme . L-threonine aldolase in a slug-flow microfluidic system. Slug-flow arrangement allows for the continuous refilling of sparingly soluble substrate (benzaldehyde) into an aqueous reaction mixture. We identified suitable composition of an

  15. Diastereoselective and one-pot synthesis of trans-isoquinolonic acids via three-component condensation of homophthalic anhydride, aldehydes, and ammonium acetate catalyzed by aspartic acid

    Czech Academy of Sciences Publication Activity Database

    Ghorbani-Choghamarani, A.; Hajjami, M.; Norouzi, M.; Abbasityula, Y.; Eigner, Václav; Dušek, Michal

    2013-01-01

    Roč. 69, č. 32 (2013), s. 6541-6544 ISSN 0040-4020 Grant - others:AVČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : isoquinolonic acid * diastereoselective * aldehyde * homophthalic anhydride * ammonium acetate Subject RIV: CC - Organic Chemistry Impact factor: 2.817, year: 2013

  16. Diastereoselective Synthesis of Novel Heterocyclic Scaffolds through Tandem Petasis 3-Component/Intramolecular Diels-Alder and ROM-RCM Reactions

    DEFF Research Database (Denmark)

    Ishøy, Mette; Petersen, Rico; Petersen, Michael Åxman

    2017-01-01

    A high-yielding, stereoselective and extraordinarily complexity generatingPetasis 3-component/intramolecular Diels-Alderreaction has been developed. In combination with ROM-RCM, rapid access to complex sp3-rich heterocyclic scaffolds amenableto subsequent functionalization and library synthesis...

  17. Highly enantio- and diastereoselective synthesis of β-methyl-γ- monofluoromethyl-substituted alcohols

    KAUST Repository

    Yang, Wenguo

    2011-06-07

    Enanatiopure β-methyl-γ-monofluoromethyl alcohols were prepared from the allylic alkylation between fluorobis(phenylsulfonyl)methane with Morita-Baylis-Hillman carbonates. The reaction was catalyzed by using the Cinchona alkaloid derivative, (DHQD)2AQN. The origin of the stereoselectivity was verified by DFT methods. Calculated geometries and relative energies of various transition states strongly support the observed stereoselectivity. © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Switchable Diastereoselectivity in the Fluoride Promoted Vinylogous Mukaiyama-Michael Reaction of 2-Trimethylsilyloxyfuran Catalyzed by Crown Ethers

    KAUST Repository

    Della Sala, Giorgio; Sicignano, Marina; Schettini, Rosaria; De Riccardis, Francesco; Cavallo, Luigi; Minenkov, Yury; Batisse, Chloé ; Hanquet, Gilles; Leroux, Frederic; IZZO, Irene

    2017-01-01

    diastereoselectivities when benzo-15-crown-5 in CH2Cl2 was employed. On the other hand, high syn-diastereoselectivities (from 76:24 to 96:4) were achieved by employing dicyclohexane-18-crown-6 in toluene. Based on DFT calculations, the catalysts

  19. Switchable Diastereoselectivity in the Fluoride Promoted Vinylogous Mukaiyama-Michael Reaction of 2-Trimethylsilyloxyfuran Catalyzed by Crown Ethers

    KAUST Repository

    Della Sala, Giorgio

    2017-05-31

    The fluoride promoted vinylogous Mukaiyama-Michael reaction (VMMR) of 2-trimethylsilyloxyfuran with diverse α,β-unsaturated ketones is described. The TBAF catalyzed VMMR afforded high anti-diastereoselectivity irrespective of the solvents used. The KF/crown ethers catalytic systems proved to be highly efficient in terms of yields and resulted in a highly diastereoselective unprecedented solvent/catalyst switchable reaction. Anti-adducts were obtained as single diastereomers or with excellent diastereoselectivities when benzo-15-crown-5 in CH2Cl2 was employed. On the other hand, high syn-diastereoselectivities (from 76:24 to 96:4) were achieved by employing dicyclohexane-18-crown-6 in toluene. Based on DFT calculations, the catalysts/solvents-dependent switchable diastereoselectivities are proposed to be the result of loose or tight cation-dienolate ion pairs.

  20. Gold-Catalyzed Enantio- and Diastereoselective Syntheses of Left Fragments of Azadirachtin/Meliacarpin-Type Limonoids.

    Science.gov (United States)

    Shi, Hang; Tan, Ceheng; Zhang, Weibin; Zhang, Zichun; Long, Rong; Gong, Jianxian; Luo, Tuoping; Yang, Zhen

    2016-02-05

    Meliacarpin-type limonoids are an important class of organic insecticides. Their syntheses are challenging due to their chemical complexity. Here, we report the highly enantio- and diastereoselective synthesis of the left fragments of azadirachtin I and 1-cinnamoylmelianolone, being two important family members of meliacarpin-type limonoids, via pairwise palladium- and gold-catalyzed cascade reactions. Gold-catalyzed reactions of 1,7-diynes were performed as model studies, and the efficient construction of tetracyclic late-stage intermediates was achieved on the basis of this key transformation. Our unique route gave both of the left fragments in 23 steps from the commercially available chiral starting material (-)-carvone. This study significantly advances research on the synthesis of the meliacarpin-type limonoids.

  1. Diastereoselective synthesis of ethyl ( Z)-3-(8-methylimidazo-[1,2- a]pyrid-2-yl)-2-phenylthioacrylate. X-ray crystal structure and conformational analysis

    Science.gov (United States)

    Gautier, A.; Roche, D.; Métin, J.; Carpy, A.; Madesclaire, M.

    1995-09-01

    The title compound 2, a gem vinyl sulfide ester, has been obtained diastereoselectively (de > 98%) by action of the ethyl thiophenoxyacetate carbanion on the imidazo[1,2- a]pyridinecarbaldehyde 1 in a basic medium, at low temperature. The X-ray crystal structure of 2 (C 19H 19N 2O 2S: Mr = 338.43, triclinic, P 1¯, a = 8.193(3) Å, b = 10.090(2) Å, c = 10.981(4) Å, α = 88.12(2)°, β = 78.66(4)°, γ = 78.53(2)°, V = 872.3(6) Å3, Z = 2, Dcalc = 1.29 g cm -3, λ( Mo Kα) = 0.71069 Å, μ = 0.189 mm -1, F(000) = 356, T = 293 K, R = 0.043 for 3610 observed reflections) has been determined and confirmed the Z configuration. The molecule is almost planar except for the phenyl ring situated in an approximate perpendicular plane. Despite the presence of the conjugate double bonds of the vinyl ester group (acrylate), coplanar with the imidazopyridine heterocycle, there is no evidence of π-electron delocalization over the whole structure. The crystal cohesion is ensured by a dense network of van der Waals contacts. A conformational analysis of the Z and E isomers by means of a Monte Carlo search and a stochastic dynamics simulation in CHCl 3 has shown that according to the method the Z isomer is more stable than the E isomer by about 7 to 10 kJ mol -1.

  2. Total Synthesis of Adunctin B.

    Science.gov (United States)

    Dethe, Dattatraya H; Dherange, Balu D

    2018-03-16

    Total synthesis of (±)-adunctin B, a natural product isolated from Piper aduncum (Piperaceae), has been achieved using two different strategies, in seven and three steps. The efficient approach features highly atom economical and diastereoselective Friedel-Crafts acylation, alkylation reaction and palladium catalyzed Wacker type oxidative cyclization.

  3. Diastereoselective and enantioselective reduction of tetralin-1,4-dione

    OpenAIRE

    Kündig, E Peter; Enriquez-Garcia, Alvaro

    2008-01-01

    Summary Background The chemistry of tetralin-1,4-dione, the stable tautomer of 1,4-dihydroxynaphthalene, has not been explored previously. It is readily accessible and offers interesting opportunities for synthesis. Results The title reactions were explored. L-Selectride reduced the diketone to give preferentially the cis-diol (d.r. 84 : 16). Red-Al gave preferentially the trans-diol (d.r. 13 : 87). NaBH4, LiAlH4, and BH3 gave lower diastereoselectivities (yields: 76–98%). Fractional crystall...

  4. Iridium-Catalyzed Dynamic Kinetic Isomerization: Expedient Synthesis of Carbohydrates from Achmatowicz Rearrangement Products.

    Science.gov (United States)

    Wang, Hao-Yuan; Yang, Ka; Bennett, Scott R; Guo, Sheng-rong; Tang, Weiping

    2015-07-20

    A highly stereoselective dynamic kinetic isomerization of Achmatowicz rearrangement products was discovered. This new internal redox isomerization provided ready access to key intermediates for the enantio- and diastereoselective synthesis of a series of naturally occurring sugars. The nature of the de novo synthesis also enables the preparation of both enantiomers. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Synthesis of Isoiminosugars

    DEFF Research Database (Denmark)

    Hyldtoft, Lene; Godskesen, Michael Anders; Lundt, Inge

    1998-01-01

    A short synthesis of isoiminosugars have been developed. Bromolactones are diastereoselectively alkylated at C-2 followed by ring closure to the corresponding lactams. Reduction of these then gives isoiminosugars......A short synthesis of isoiminosugars have been developed. Bromolactones are diastereoselectively alkylated at C-2 followed by ring closure to the corresponding lactams. Reduction of these then gives isoiminosugars...

  6. One-Pot Catalytic Enantio- and Diastereoselective Syntheses of anti-, syn-cis-Disubstituted, and syn-Vinyl Cyclopropyl Alcohols

    Science.gov (United States)

    Kim, Hun Young; Salvi, Luca; Carroll, Patrick J.; Walsh, Patrick J.

    2009-01-01

    Highly enantio- and diastereoselective methods for the synthesis of a variety of cyclopropyl alcohols are reported. These methods represent the first one-pot approaches to syn-vinyl cyclopropyl alcohols, syn-cis-disubstituted cyclopropyl alcohols, and anti-cyclopropyl alcohols from achiral precursors. The methods begin with enantioselective C–C bond formations promoted by a MIB-based zinc catalyst to generate allylic alkoxide intermediates. The intermediates are then subjected to in situ alkoxide-directed cyclopropanation to provide cyclopropyl alcohols. In the synthesis of vinyl cyclopropyl alcohols, hydroboration of enynes is followed by transmetalation of the resulting dienylborane to zinc to provide dienylzinc reagents. Enantioselective addition to aldehydes generates the requisite dienyl zinc alkoxides, which are then subjected to in situ cyclopropanation to furnish vinyl cyclopropyl alcohols. Cyclopropanation occurs at the double bond allylic to the alkoxide. Using this method, syn-vinylcyclopropyl alcohols are obtained in 65–85% yield, 76–93% ee, and >19:1 dr. To prepare anti-cyclopropanols, enantioselective addition of alkylzinc reagents to conjugated enals provides allylic zinc alkoxides. Because direct cyclopropanation provides syn-cyclopropyl alcohols, the intermediate allylic alkoxides were treated with TMSCl/Et3N to generate intermediate silyl ethers. In situ cyclopropanation of the allylic silyl ether resulted in cyclopropanation to form the anti-cyclopropyl silyl ether. Workup with TBAF affords the anti-cyclopropyl alcohols in one-pot in 60–82% yield, 89–99% ee, and ≥10:1 dr. For the synthesis of cis-disubstituted cyclopropyl alcohols, in situ generated (Z)-vinyl zinc reagents were employed in asymmetric addition to aldehydes to generate (Z)-allylic zinc alkoxides. In situ cyclopropanation provides syn-cis-disubstituted cyclopropyl alcohols in 42–70% yield, 88–97% ee, and >19:1 dr. These one-pot procedures enable the synthesis of a

  7. Diastereoselective synthesis of pyridyl substituted thiazolidin-4-ones. New ligands for the Cu(I) catalyzed asymmetric conjugate addition of diethylzinc to enones

    NARCIS (Netherlands)

    Vries, André H.M. de; Hof, Robert P.; Staal, Danny; Kellogg, Richard M.; Feringa, Bernard

    1997-01-01

    Several novel thiazolidin-4-ones have been synthesized from chiral non-racemic alpha-mercapto acids by a three component reaction in high yields and with diastereomeric excesses up to 91%. After recrystallization, the thiazolidinones were obtained diastereomerically pure and were employed as chiral

  8. Inversion of Configuration at the Phosphorus Nucleophile in the Diastereoselective and Enantioselective Synthesis of P-Stereogenic syn-Phosphiranes from Chiral Epoxides.

    Science.gov (United States)

    Muldoon, Jake A; Varga, Balázs R; Deegan, Meaghan M; Chapp, Timothy W; Eördögh, Ádám M; Hughes, Russell P; Glueck, David S; Moore, Curtis E; Rheingold, Arnold L

    2018-04-23

    Nucleophilic substitution results in inversion of configuration at the electrophilic carbon center (S N 2) or racemization (S N 1). The stereochemistry of the nucleophile is rarely considered, but phosphines, which have a high barrier to pyramidal inversion, attack electrophiles with retention of configuration at P. Surprisingly, cyclization of bifunctional secondary phosphine alkyl tosylates proceeded under mild conditions with inversion of configuration at the nucleophile to yield P-stereogenic syn-phosphiranes. DFT studies suggested that the novel stereochemistry results from acid-promoted tosylate dissociation to yield an intermediate phosphenium-bridged cation, which undergoes syn-selective cyclization. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Nazarov cyclization initiated by peracid oxidation: the total synthesis of (+/-)-rocaglamide.

    Science.gov (United States)

    Malona, John A; Cariou, Kevin; Frontier, Alison J

    2009-06-10

    The total syntheses of aglafolin, rocagloic acid, and rocaglamide using Nazarov cyclization are described. Generation of the necessary oxyallyl cation intermediate was accomplished via peracid oxidation of an allenol ether to generate an unusual oxycarbenium ion species that undergoes cyclization. The synthesis is efficient, highly diastereoselective, and strategically distinct from previous syntheses of rocaglamide.

  10. Diastereoselectivity in scalemic tartrate/titanium epoxidations.

    Science.gov (United States)

    Brown, J M; Leppard, S J; Oakes, J; Thornthwaite, D

    2000-06-01

    Nonlinearity in the diastereoselectivity of epoxidation of allylic alcohols with mixtures of titanium isopropoxide, tertbutyl hydroperoxide, and diethyl tartrate was observed. Racemic and enantiomerically pure alcohols E-2-methyl-4-hexen-3-ol and E-1-methoxy-5-(O-tertbutyldimethylsilyloxy)-2-penten-4-ol were prepared. Epoxidation reactions were carried out with Ti(OPri)4 and ButOOH accompanied by diethyl tartrate of varying enantiomeric purity. The simplest explanation of these results is that a dimeric epoxidation reagent is involved, with significantly different reactivity for the homochiral and racemic forms. Copyright 2000 Wiley-Liss, Inc.

  11. Acyclic diastereoselection in prochiral radical addition to prochiral olefins.

    Science.gov (United States)

    Sibi, Mukund P; Rheault, Tara R; Chandramouli, Sithamalli V; Jasperse, Craig P

    2002-03-27

    The stereochemical preference (syn or anti) when prochiral radicals add to prochiral acceptors is of fundamental interest. The primary focus of this research was to determine which factors influence the relative stereochemistry between the beta and gamma chiral centers when these are formed concurrently. While moderate diastereoselectivity was found for addition of alkyl (6a-d) and alpha-alkoxy radicals (16a-c) (15:1 anti). Steric influence in alkyl radical additions was difficult to evaluate due to decreased reactivity when using bulky reaction partners; however, more reactive alpha-alkoxy radicals, it was found that increasing steric bulk leads to moderate increases in selectivity. In addition, higher selectivity was observed when employing lanthanide Lewis acids whose environment (reactivity) was modified using achiral additives, suggesting a potentially simple means for selectivity enhancements in radical reactions. Overall these results indicate that significant stereoelectronic effects are necessary to achieve high levels of selectivity in prochiral radical additions to prochiral acceptors.

  12. The Inverse Demand Oxa-Diels-Alder Reaction of Resorcinarenes: An Experimental and Theoretical Analysis of Regioselectivity and Diastereoselectivity.

    Science.gov (United States)

    Stefańska, Karolina; Jędrzejewska, Hanna; Wierzbicki, Michał; Szumna, Agnieszka; Iwanek, Waldemar

    2016-07-15

    The Diels-Alder reaction enables introduction of new functionalities onto the resorcinarene skeleton with simultaneous generation of new stereogenic centers and expansion of the internal cavity. We present highly regio- and diastereoselective inverse electron demand oxa-Diels-Alder reactions of resorcinarene ortho-quinone methide with benzofuran and indene, each generating 12 new stereogenic centers. The mechanism and reasons for regioselectivity and diastereoselectivity were analyzed using theoretical calculations (NBO charges, Fukui functions, transition state energies, and thermodynamic stability of the products). Enantiomers were separated, and their configurations were determined by comparison of experimental and theoretical electronic circular dichroism spectra.

  13. Stereoselective total synthesis of the potent anti-asthmatic compound CMI-977 (LDP-977)

    Energy Technology Data Exchange (ETDEWEB)

    Dias, Luiz Carlos; Farina, Lui Strambi; Ferreira, Marco Antonio Barbosa, E-mail: ldias@iqm.unicamp.br [Universidade de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica

    2013-02-15

    A short and efficient stereoselective total synthesis of CMI-977 (LDP-977), a potent and orally active anti-asthmatic compound, was developed. The key steps involve a highly diastereoselective Mukaiyama oxidative cyclization, which provides the trans-THF (tetrahydrofuran) unit and a Seyferth-Gilbert homologation to construct the triple bond in the target molecule. The synthesis of the key chiral building block was performed using Jacobsen hydrolytic kinetic resolution. (author)

  14. Efficient Asymmetric Synthesis of S,S-2-methylsulfanyl-2-methylsulfinyl-1-indanone

    OpenAIRE

    Derisvaldo Rosa Paiva; Roberto da Silva Gomes

    2013-01-01

    Diastereoselective synthesis of SS-2-methylsulfanyl-2-methylsulfinyl-1-indanol by reduction of SS-2-methylsulfanyl-2-methylsulfinyl-1-indanone optically enriched demonstrating to be highly efficiency using the sulfanyl group as asymmetric induction control agent during an addition reaction to carbonyl group.The 2-methylsulfinyl-1-indanone was obtained for the first time in one unique step without further oxidation steps. The synthesis of SR, SS of 2-methylsulphinyl-1-indanone optically enrich...

  15. Stereoselective total synthesis of the potent anti-asthmatic compound CMI-977 (LDP-977)

    International Nuclear Information System (INIS)

    Dias, Luiz Carlos; Farina, Lui Strambi; Ferreira, Marco Antonio Barbosa

    2013-01-01

    A short and efficient stereoselective total synthesis of CMI-977 (LDP-977), a potent and orally active anti-asthmatic compound, was developed. The key steps involve a highly diastereoselective Mukaiyama oxidative cyclization, which provides the trans-THF (tetrahydrofuran) unit and a Seyferth-Gilbert homologation to construct the triple bond in the target molecule. The synthesis of the key chiral building block was performed using Jacobsen hydrolytic kinetic resolution. (author)

  16. Diastereoselective and enantioselective conjugate addition reactions utilizing α,β-unsaturated amides and lactams

    Directory of Open Access Journals (Sweden)

    Katherine M. Byrd

    2015-04-01

    Full Text Available The conjugate addition reaction has been a useful tool in the formation of carbon–carbon bonds. The utility of this reaction has been demonstrated in the synthesis of many natural products, materials, and pharmacological agents. In the last three decades, there has been a significant increase in the development of asymmetric variants of this reaction. Unfortunately, conjugate addition reactions using α,β-unsaturated amides and lactams remain underdeveloped due to their inherently low reactivity. This review highlights the work that has been done on both diastereoselective and enantioselective conjugate addition reactions utilizing α,β-unsaturated amides and lactams.

  17. A Short Synthesis of (+)-Cyclophellitol

    DEFF Research Database (Denmark)

    Hansen, Flemming Gundorph; Bundgaard, Eva; Madsen, Robert

    2005-01-01

    A new synthesis of (+)-cyclophellitol, a potent b-glucosidase inhibitor, has been completed in nine steps from D-xylose. The key transformations involve a zinc-mediated fragmentation of benzyl-protected methyl 5-deoxy-5-iodo-xylofuranoside followed by a highly diastereoselective indium-mediated c......-mediated coupling with ethyl 4-bromocrotonate. Subsequent ring-closing olefin metathesis, ester reduction, olefin epoxidation, and deprotection then afford the natural product. This constitutes the shortest synthesis of (+)-cyclophellitol reported to date....

  18. N-Heterocyclic-Carbene-Catalysed Diastereoselective Vinylogous Mukaiyama/Michael Reaction of 2-(Trimethylsilyloxy)furan and Enones

    KAUST Repository

    Wang, Ying; Du, Guang Fen; Xing, Fen; Huang, Kuo-Wei; Dai, Bin; He, Lin

    2015-01-01

    N-heterocyclic carbenes have been utilised as highly efficient nucleophilic organocatalysts to mediate vinylogous Mukaiyama/Michael reactions of 2-(trimethylsilyloxy)furan with enones to afford γ-substituted butenolides in 44-99% yield with 3:1-32:1 diastereoselectivity. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. N-Heterocyclic-Carbene-Catalysed Diastereoselective Vinylogous Mukaiyama/Michael Reaction of 2-(Trimethylsilyloxy)furan and Enones

    KAUST Repository

    Wang, Ying

    2015-10-15

    N-heterocyclic carbenes have been utilised as highly efficient nucleophilic organocatalysts to mediate vinylogous Mukaiyama/Michael reactions of 2-(trimethylsilyloxy)furan with enones to afford γ-substituted butenolides in 44-99% yield with 3:1-32:1 diastereoselectivity. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Stereoselective, nitro-Mannich/lactamisation cascades for the direct synthesis of heavily decorated 5-nitropiperidin-2-ones and related heterocycles

    Directory of Open Access Journals (Sweden)

    Pavol Jakubec

    2012-04-01

    Full Text Available A versatile nitro-Mannich/lactamisation cascade for the direct stereoselective synthesis of heavily decorated 5-nitropiperidin-2-ones and related heterocycles has been developed. A highly enantioenriched substituted 5-nitropiperidin-2-one was synthesised in a four component one-pot reaction combining an enantioselective organocatalytic Michael addition with the diastereoselective nitro-Mannich/lactamisation cascade. Protodenitration and chemoselective reductive manipulation of the heterocycles was used to install contiguous and fully substituted stereocentres in the synthesis of substituted piperidines.

  1. Inverting the diastereoselectivity of the mukaiyama-michael addition with graphite-based catalysts

    KAUST Repository

    Acocella, Maria Rosaria; Mauro, Marco; Falivene, Laura; Cavallo, Luigi; Guerra, Gaetano

    2014-01-01

    , the graphite-based catalysts described here invert the diastereoselectivity relative to that observed with known catalysts, with the unprecedented large prevalence of the anti diastereoisomer. This inverted diastereoselectivity is increased when the catalyst

  2. Cyclopropenes in Metallacycle-Mediated Cross-Coupling with Alkynes: Convergent Synthesis of Highly Substituted Vinylcyclopropanes.

    Science.gov (United States)

    O'Rourke, Natasha F; Micalizio, Glenn C

    2016-03-18

    Stereodivergent metallacycle-mediated cross-coupling reactions are described for the synthesis of densely functionalized vinylcyclopropanes from the union of alkynes with cyclopropenes. Strategies explored include hydroxyl-directed and nondirected processes, with the latter of these delivering vinylcyclopropanes with exquisite levels of regio- and stereoselectivity. Challenges inherent to these coupling reactions include diastereoselectivity (with respect to the cyclopropene) and regioselectivity (with respect to both coupling partners).

  3. Catalytic stereoselective synthesis of highly substituted indanones via tandem Nazarov cyclization and electrophilic fluorination trapping.

    Science.gov (United States)

    Nie, Jing; Zhu, Hong-Wei; Cui, Han-Feng; Hua, Ming-Qing; Ma, Jun-An

    2007-08-02

    A new catalytic stereoselective tandem transformation via Nazarov cyclization/electrophilic fluorination has been accomplished. This sequence is efficiently catalyzed by a Cu(II) complex to afford fluorine-containing 1-indanone derivatives with two new stereocenters with high diastereoselectivity (trans/cis up to 49/1). Three examples of catalytic enantioselective tandem transformation are presented.

  4. Highly selective sulfur ylide mediated asymmetric epoxidations and aziridinations using an inexpensive chiral sulfide and applications to the synthesis of quinine and quinidine (abstract)

    International Nuclear Information System (INIS)

    Arshad, M.; Illa, O.; Mcgarrigle, E.M.

    2011-01-01

    Asymmetric sulfur ylide mediated epoxidation, which is considered a complimentary method to asymmetric epoxidation of alkene has been utilized as a key step in the asymmetric total synthesis of complex cinchona alkaloids quinine and quinidine. Isothiocineole 1, which was readily available in one step from very inexpensive starting materials, is employed as a chiral sulfide to prepare the desired sulfonium salt 2. The semi-stabilised ylide derived from this salt on epoxidation with meroquinene aldehyde 3, afforded the required epoxide 4 in 81% yield and 89:11 diastereoselectivity (trans/cis). The epoxide was converted to the target quinine 5 in 73% yield over four steps in one pot. Similarly, the opposite enantiomer of isothiocineole was used to synthesise the corresponding sulfonium salt, which on reaction with meroquinene aldehyde gave epoxide in 73% yield and 84:16 diastereoselectivity (trans/cis). This epoxide was transformed to the target quinidine in 78% yield over four steps in one pot. The epoxidation reactions proceeded under reagent control with high trans selectivity. The effect of sulfide and ylide substituents on the stereochemical outcome of the epoxidation reaction is also prescribed. (author)

  5. Highly regio- and diastereoselective, acidic clay supported intramolecular nitrile oxide-alkene cycloaddition on D-ribose derived nitriles: an efficient synthetic route to isoxazoline fused five and six membered carbocycles.

    Science.gov (United States)

    Panda, Amarendra; Das, Sulagna; Pal, Shantanu

    2014-10-29

    An efficient synthetic route to isoxazoline fused carbocycles from carbohydrate scaffolds that comprise of free hydroxyl group(s) is described with high regio- and stereoselectivity. Montmorillonite K-10/chloramine T oxidation and in situ intramolecular nitrile oxide-alkene cycloaddition (INOC) of D-ribose derived oximes have been developed for the diversity oriented synthesis of isoxazoline fused five and six membered carbocycles. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides

    OpenAIRE

    Camozzato, Andreza C.; Tenius, Beatriz S. M.; Oliveira, Eduardo R. de; Viegas Jr., Cláudio; Victor, Maurício M.; Silveira, Leandro G. da

    2008-01-01

    Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride®) in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring.

  7. Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides

    International Nuclear Information System (INIS)

    Camozzato, Andreza C.; Tenius, Beatriz S. M.; Oliveira, Eduardo R. de; Viegas Junior, Claudio; Victor, Mauricio M.; Silveira, Leandro G. da

    2008-01-01

    Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride R ) in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring. (author)

  8. Metal-free, mild, nonepimerizing, chemo- and enantio- or diastereoselective N-alkylation of amines by alcohols via oxidation/imine-iminium formation/reductive amination: a pragmatic synthesis of octahydropyrazinopyridoindoles and higher ring analogues.

    Science.gov (United States)

    Khan, Imran A; Saxena, Anil K

    2013-12-06

    A mild step and atom-economical nonepimerizing chemo- and enantioselective N-alkylating procedure has been developed via oxidation/imine-iminium formation/reduction cascade using TEMPO-BAIB-HEH-Brønsted acid catalysis in DMPU as solvent and a stoichiometric amount of amine. The optimized conditions were further extended for the nonenzymatic kinetic resolution of the chiral amine thus formed under nonenzymatic in situ hydrogen-transfer conditions using VAPOL-derived phosphoric acid (VAPOL-PA) as the Brønsted acid catalyst. The enantioselective cascade of the presented reaction was successfully utilized in the synthesis of octahydropyrazinopyridoindole and its higher ring analogues.

  9. RPython high-level synthesis

    Science.gov (United States)

    Cieszewski, Radoslaw; Linczuk, Maciej

    2016-09-01

    The development of FPGA technology and the increasing complexity of applications in recent decades have forced compilers to move to higher abstraction levels. Compilers interprets an algorithmic description of a desired behavior written in High-Level Languages (HLLs) and translate it to Hardware Description Languages (HDLs). This paper presents a RPython based High-Level synthesis (HLS) compiler. The compiler get the configuration parameters and map RPython program to VHDL. Then, VHDL code can be used to program FPGA chips. In comparison of other technologies usage, FPGAs have the potential to achieve far greater performance than software as a result of omitting the fetch-decode-execute operations of General Purpose Processors (GPUs), and introduce more parallel computation. This can be exploited by utilizing many resources at the same time. Creating parallel algorithms computed with FPGAs in pure HDL is difficult and time consuming. Implementation time can be greatly reduced with High-Level Synthesis compiler. This article describes design methodologies and tools, implementation and first results of created VHDL backend for RPython compiler.

  10. Total synthesis of broussonetine F: the orthoamide Overman rearrangement of an allylic diol.

    Science.gov (United States)

    Hama, Naoto; Aoki, Toshihiro; Miwa, Shohei; Yamazaki, Miki; Sato, Takaaki; Chida, Noritaka

    2011-02-18

    A first total synthesis of broussonetine F from diethyl L-tartrate was achieved. The cornerstone of our synthesis was an orthoamide Overman rearrangement, which provided an allylic amino alcohol with complete diastereoselectivity.

  11. A 11-Steps Total Synthesis of Magellanine through a Gold(I)-Catalyzed Dehydro Diels-Alder Reaction.

    Science.gov (United States)

    McGee, Philippe; Bétournay, Geneviève; Barabé, Francis; Barriault, Louis

    2017-05-22

    We have developed an innovative strategy for the formation of angular carbocycles via a gold(I)-catalyzed dehydro Diels-Alder reaction. This transformation provides rapid access to a variety of complex angular cores in excellent diastereoselectivities and high yields. The usefulness of this Au I -catalyzed cycloaddition was further demonstrated by accomplishing a 11-steps total synthesis of (±)-magellanine. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Cross-Aldol Reaction of Activated Carbonyls with Nitrosocarbonyl Intermediates: Stereoselective Synthesis toward α-Hydroxy-β-amino Esters and Amides.

    Science.gov (United States)

    Mallik, Sumitava; Bhajammanavar, Vinod; Ramakrishna, Isai; Baidya, Mahiuddin

    2017-07-21

    A practical and flexible strategy toward α-hydroxy-β-amino esters and amides, which are important biological motifs, based on an organocatalytic cross-aldol reaction of in situ-generated nitrosocarbonyl intermediates followed by hydrogenation is presented. The protocol features operational simplicity, high yields, a wide substrate scope, and high regio- and diastereoselectivity profiles. The utility of this method was showcased through the synthesis of bestatin analogues and indole formation.

  13. Catalytic Asymmetric Piancatelli Rearrangement: Brønsted Acid Catalyzed 4π Electrocyclization for the Synthesis of Multisubstituted Cyclopentenones

    KAUST Repository

    Cai, Yunfei

    2016-10-13

    The first catalytic asymmetric Piancatelli reaction is reported. Catalyzed by a chiral Brønsted acid, the rearrangement of a wide range of furylcarbinols with a series of aniline derivatives provides valuable aminocyclopentenones in high yields as well as excellent enantioselectivities and diastereoselectivities. The high value of the aza-Piancatelli rearrangement was demonstrated by the synthesis of a cyclopentane-based hNK1 antagonist analogue.

  14. Stereoselective Synthesis of Highly Functionalized α-Diazo-β-ketoalkanoates via Catalytic Onepot Mukaiyama-Aldol Reactions

    Science.gov (United States)

    Zhou, Lei; Doyle, Michael P.

    2010-01-01

    Methyl diazoacetoacetate undergoes zinc triflate catalyzed condensation with a broad selection of aldehydes to produce δ-siloxy-α-diazo-β-ketoalkanoates in good yield, and δ-hydroxy-α-diazo-β-ketoalkanoates are formed with high diastereoselectivity in reactions with α-diazo-β-ketopentanoate promoted by dibutylboron triflate. PMID:20102172

  15. Diastereoselective Flexible Synthesis of Carbocyclic C-Nucleosides

    Czech Academy of Sciences Publication Activity Database

    Maier, L.; Khirsariya, P.; Hylse, O.; Adla, S.K.; Cernova, L.; Poljak, M.; Krajčovičová, S.; Weis, E.; Drápela, Stanislav; Souček, Karel; Paruch, K.

    2017-01-01

    Roč. 82, č. 7 (2017), s. 3382-3402 ISSN 0022-3263 Institutional support: RVO:68081707 Keywords : mitsunobu * catalysis * alcohols Subject RIV: CC - Organic Chemistry OBOR OECD: Organic chemistry Impact factor: 4.849, year: 2016

  16. Synthesis of high luminescent carbon nanoparticles

    Science.gov (United States)

    Gvozdyuk, Alina A.; Petrova, Polina S.; Goryacheva, Irina Y.; Sukhorukov, Gleb B.

    2017-03-01

    In this article we report an effective and simple method for synthesis of high luminescent carbon nanodots (CDs). In our work as a carbon source sodium dextran sulfate (DS) was used because it is harmless, its analogs are used in medicine as antithrombotic compounds and blood substitutes after hemorrhage. was used as a substrate We investigated the influence of temperature parameters of hydrothermal synthesis on the photoluminescence (PL) intensity and position of emission maxima. We discovered that the PL intensity can be tuned by changing of synthesis temperature and CD concentration.

  17. Efficient Asymmetric Synthesis of S,S-2-methylsulfanyl-2-methylsulfinyl-1-indanone

    Directory of Open Access Journals (Sweden)

    Derisvaldo Rosa Paiva

    2013-05-01

    Full Text Available Diastereoselective synthesis of SS-2-methylsulfanyl-2-methylsulfinyl-1-indanol by reduction of SS-2-methylsulfanyl-2-methylsulfinyl-1-indanone optically enriched demonstrating to be highly efficiency using the sulfanyl group as asymmetric induction control agent during an addition reaction to carbonyl group.The 2-methylsulfinyl-1-indanone was obtained for the first time in one unique step without further oxidation steps. The synthesis of SR, SS of 2-methylsulphinyl-1-indanone optically enriched in good yield and good enantiomeric excess determined by nuclear magnetic resonance technique employing the Kagan reagent as chiral shift agent.

  18. Diastereoselective formation of metallamacrocyclic (arene)Ru(II) and CpRh(III) complexes.

    Science.gov (United States)

    Lehaire, Marie-Line; Scopelliti, Rosario; Herdeis, Lorenz; Polborn, Kurt; Mayer, Peter; Severin, Kay

    2004-03-08

    The reaction of [(arene)RuCl(2)](2) (arene = cymene, 1,3,5-C(6)H(3)Me(3)) and [CpRhCl(2)](2) half-sandwich complexes with tridentate heterocyclic ligands in the presence of base has been investigated. In all cases, the chloro-ligands were substituted to give metallacyclic products with ring sizes between 4 and 18 atoms. The cyclization occurs in a highly diastereoselective fashion with chiral recognition between the different metal fragments. The complexes were comprehensively characterized by elemental analysis, NMR spectroscopy, and single crystal X-ray crystallography. For 2-hydroxy-nicotinic acid and 2-amino-nicotinic acid, dinuclear structures were obtained (15-17) whereas for 2,3-dihydroxyquinoline, 2,3-dihydroxyquinoxaline, and 6-methyl-2,3-phenazinediol, trimeric assemblies were found (19-22), and for 4-imidazolecarboxylic acid, a tetrameric assembly (18) was found.

  19. Synthesis of the AB ring system of clifednamide utilizing Claisen rearrangement and Diels-Alder reaction as key steps.

    Science.gov (United States)

    Loke, Inga; Bentzinger, Guillaume; Holz, Julia; Raja, Aruna; Bhasin, Aman; Sasse, Florenz; Köhn, Andreas; Schobert, Rainer; Laschat, Sabine

    2016-01-21

    In order to construct the functionalized AB ring system of clifednamide, member of the class of macrocyclic tetramic acid lactams, a synthesis was developed which utilized an Ireland-Claisen rearrangement and an intramolecular Diels-Alder reaction. Starting from di-O-isopropylidene-d-mannitol the allyl carboxylate precursor for the sigmatropic rearrangement was prepared. This rearrangement proceeded diastereoselectively only in the presence of an allyl silyl ether instead of the parent enone in the side chain, as suggested by deuteration experiments. A subsequent Diels-Alder reaction yielded the target ethyl hexahydro-1H-indene-carboxylate with high diastereoselectivity. Quantum-chemical investigations of this intramolecular Diels-Alder reaction support the proposed configuration of the final product.

  20. Liquid-assisted grinding and ion pairing regulates percentage conversion and diastereoselectivity of the Wittig reaction under mechanochemical conditions.

    Science.gov (United States)

    Denlinger, Kendra Leahy; Ortiz-Trankina, Lianna; Carr, Preston; Benson, Kingsley; Waddell, Daniel C; Mack, James

    2018-01-01

    Mechanochemistry is maturing as a discipline and continuing to grow, so it is important to continue understanding the rules governing the system. In a mechanochemical reaction, the reactants are added into a vessel along with one or more grinding balls and the vessel is shaken at high speeds to facilitate a chemical reaction. The dielectric constant of the solvent used in liquid-assisted grinding (LAG) and properly chosen counter-ion pairing increases the percentage conversion of stilbenes in a mechanochemical Wittig reaction. Utilizing stepwise addition/evaporation of ethanol in liquid-assisted grinding also allows for the tuning of the diastereoselectivity in the Wittig reaction.

  1. Total synthesis of (±)-antroquinonol d.

    Science.gov (United States)

    Sulake, Rohidas S; Jiang, Yan-Feng; Lin, Hsiao-Han; Chen, Chinpiao

    2014-11-21

    Total synthesis of (±)-antroquinonol D, which is isolated from very expensive and rarely found Antrodia camphorata and which has potential anticancer properties, was achieved from 4-methoxyphenol. In addition, a Michael addition to dimethoxy cyclohexadienones was studied. The main step involved chelation and substrate-controlled diastereoselective reduction of cyclohexenone and lactonization. Lactone synthesis facilitated the diastereoselective reduction of ketone, which help control the desired stereochemistry at the crucial stereogenic center in the natural product. Other key reactions in the synthesis involved a Michael addition of dimethyl malonate on cyclohexadienone, dihydroxylation, and Wittig olefination. A sesquiterpene side chain was synthesized through coupling with geranyl phenyl sulfide and Bouveault-Blanc reduction.

  2. High chemoselectivity in the phenol synthesis

    Directory of Open Access Journals (Sweden)

    A. Stephen K. Hashmi

    2011-06-01

    Full Text Available Efforts to trap early intermediates of the gold-catalyzed phenol synthesis failed. Neither inter- nor intramolecularly offered vinyl groups, ketones or alcohols were able to intercept the gold carbenoid species. This indicates that the competing steps of the gold-catalyzed phenol synthesis are much faster than the steps of the interception reaction. In the latter the barrier of activation is higher. At the same time this explains the high tolerance of this very efficient and general reaction towards functional groups.

  3. Catalyst-Directed Diastereoselective Isomerization of Allylic Alcohols for the Stereoselective Construction of C(20) in Steroid Side Chains: Scope and Topological Diversification.

    Science.gov (United States)

    Li, Houhua; Mazet, Clément

    2015-08-26

    The stereoselective construction of C20 in steroidal derivatives by a highly diastereoselective Ir-catalyzed isomerization of primary allylic alcohols is reported. A key aspect of this strategy is a straightforward access to geometrically pure steroidal enol tosylate and enol triflate intermediates for subsequent high yielding stereoretentive Negishi cross-coupling reactions to allow structural diversity to be introduced. A range of allylic alcohols participates in the diastereoselective isomerization under the optimized reaction conditions. Electron-rich and electron-poor aryl or heteroaryl substituents are particularly well-tolerated, and the stereospecific nature of the reaction provides indifferently access to the natural C20-(R) and unnatural C20-(S) configurations. Alkyl containing substrates are more challenging as they affect regioselectivity of iridium-hydride insertion. A rationale for the high diastereoselectivities observed is proposed for aryl containing precursors. The scope of our method is further highlighted through topological diversification in the side chain and within the polycyclic domain of advanced and complex steroidal architectures. These findings have the potential to greatly simplify access to epimeric structural analogues of important steroid scaffolds for applications in biological, pharmaceutical, and medical sciences.

  4. Catalytic asymmetric synthesis of the alkaloid (+)-myrtine

    NARCIS (Netherlands)

    Pizzuti, Maria Gabriefla; Minnaard, Adriaan J.; Feringa, Ben L.

    2008-01-01

    A new protocol for the asymmetric synthesis of trans-2,6-disubstituted-4-piperidones has been developed using a catalytic enantioselective conjugate addition reaction in combination with a diastereoselective lithiation-substitution sequence; an efficient synthesis of (+)-myrtine has been achieved

  5. Electrochemical synthesis of highly crystalline copper nanowires

    International Nuclear Information System (INIS)

    Kaur, Amandeep; Gupta, Tanish; Kumar, Akshay; Kumar, Sanjeev; Singh, Karamjeet; Thakur, Anup

    2015-01-01

    Copper nanowires were fabricated within the pores of anodic alumina template (AAT) by template synthesis method at pH = 2.9. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to investigate the structure, morphology and composition of fabricated nanowires. These characterizations revealed that the deposited copper nanowires were highly crystalline in nature, dense and uniform. The crystalline copper nanowires are promising in application of future nanoelectronic devices and circuits

  6. Total synthesis of a CD-ring: side-chain building block for preparing 17-epi-calcitriol derivatives from the Hajos-Parrish dione.

    Science.gov (United States)

    Michalak, Karol; Wicha, Jerzy

    2011-08-19

    An efficient synthesis of the key building block for 17-epi-calctriol from the Hajos-Parrish dione involving a sequence of diastereoselective transformation of the azulene core and the side-chain construction is presented.

  7. Asymmetric synthesis of quaternary aryl amino acid derivatives via a three-component aryne coupling reaction

    Directory of Open Access Journals (Sweden)

    Elizabeth P. Jones

    2011-11-01

    Full Text Available A method was developed for the synthesis of α-alkyl, α-aryl-bislactim ethers in good to excellent yields and high diastereoselectivities, consisting of a facile one-pot procedure in which the aryl group is introduced by means of a nucleophilic addition to benzyne and the alkyl group by alkylation of a resultant benzylic anion. Hydrolysis of the sterically less hindered adducts gave the corresponding quaternary amino acids with no racemization, whereas hydrolytic ring opening gave the corresponding valine dipeptides from bulkier bislactims.

  8. Advanced asymmetric synthesis of (1R,2S)-1-amino-2-vinylcyclopropanecarboxylic acid by alkylation/cyclization of newly designed axially chiral Ni(II) complex of glycine Schiff base.

    Science.gov (United States)

    Kawashima, Aki; Shu, Shuangjie; Takeda, Ryosuke; Kawamura, Akie; Sato, Tatsunori; Moriwaki, Hiroki; Wang, Jiang; Izawa, Kunisuke; Aceña, José Luis; Soloshonok, Vadim A; Liu, Hong

    2016-04-01

    Asymmetric synthesis of (1R,2S)-1-amino-2-vinylcyclopropanecarboxylic acid (vinyl-ACCA) is in extremely high demand due to the pharmaceutical importance of this tailor-made, sterically constrained α-amino acid. Here we report the development of an advanced procedure for preparation of the target amino acid via two-step SN2 and SN2' alkylation of novel axially chiral nucleophilic glycine equivalent. Excellent yields and diastereoselectivity coupled with reliable and easy scalability render this method of immediate use for practical synthesis of (1R,2S)-vinyl-ACCA.

  9. Inverting the diastereoselectivity of the mukaiyama-michael addition with graphite-based catalysts

    KAUST Repository

    Acocella, Maria Rosaria

    2014-02-07

    Here, we show that graphite-based catalysts, mainly graphite oxide (GO) and exfoliated GO, are effective recyclable catalysts for a relevant stereoselective Mukaiyama-Michael addition, outperforming currently available catalysts. Moreover, the graphite-based catalysts described here invert the diastereoselectivity relative to that observed with known catalysts, with the unprecedented large prevalence of the anti diastereoisomer. This inverted diastereoselectivity is increased when the catalyst concentration is reduced and after catalyst recycling. Density functional theory calculations suggest that the selectivity is determined by two types of supramolecular interactions operating between the catalyst and the substrates at the diastereoselectivity- determining transition state, specifically, the π-stacking of b-nitrostyrene with graphite and the van der Waals interaction between the SiMe3 group of the silyl ether and the graphite. © 2013 American Chemical Society.

  10. Highly reproducible polyol synthesis for silver nanocubes

    Science.gov (United States)

    Han, Hye Ji; Yu, Taekyung; Kim, Woo-Sik; Im, Sang Hyuk

    2017-07-01

    We could synthesize the Ag nanocubes highly reproducibly by conducting the polyol synthesis using HCl etchant in dark condition because the photodecomposition/photoreduction of AgCl nanoparticles formed at initial reaction stage were greatly depressed and consequently the selective self-nucleation of Ag single crystals and their selective growth reaction could be promoted. Whereas the reproducibility of the formation of Ag nanocubes were very poor when we synthesize the Ag nanocubes in light condition due to the photoreduction of AgCl to Ag.

  11. Python based high-level synthesis compiler

    Science.gov (United States)

    Cieszewski, Radosław; Pozniak, Krzysztof; Romaniuk, Ryszard

    2014-11-01

    This paper presents a python based High-Level synthesis (HLS) compiler. The compiler interprets an algorithmic description of a desired behavior written in Python and map it to VHDL. FPGA combines many benefits of both software and ASIC implementations. Like software, the mapped circuit is flexible, and can be reconfigured over the lifetime of the system. FPGAs therefore have the potential to achieve far greater performance than software as a result of bypassing the fetch-decode-execute operations of traditional processors, and possibly exploiting a greater level of parallelism. Creating parallel programs implemented in FPGAs is not trivial. This article describes design, implementation and first results of created Python based compiler.

  12. High rate flame synthesis of highly crystalline iron oxide nanorods

    International Nuclear Information System (INIS)

    Merchan-Merchan, W; Taylor, A M; Saveliev, A V

    2008-01-01

    Single-step flame synthesis of iron oxide nanorods is performed using iron probes inserted into an opposed-flow methane oxy-flame. The high temperature reacting environment of the flame tends to convert elemental iron into a high density layer of iron oxide nanorods. The diameters of the iron oxide nanorods vary from 10 to 100 nm with a typical length of a few microns. The structural characterization performed shows that nanorods possess a highly ordered crystalline structure with parameters corresponding to cubic magnetite (Fe 3 O 4 ) with the [100] direction oriented along the nanorod axis. Structural variations of straight nanorods such as bends, and T-branched and Y-branched shapes are frequently observed within the nanomaterials formed, opening pathways for synthesis of multidimensional, interconnected networks

  13. High-deposition-rate ceramics synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Allendorf, M.D.; Osterheld, T.H.; Outka, D.A. [Sandia National Laboratories, Livermore, CA (United States)] [and others

    1995-05-01

    Parallel experimental and computational investigations are conducted in this project to develop validated numerical models of ceramic synthesis processes. Experiments are conducted in the High-Temperature Materials Synthesis Laboratory in Sandia`s Combustion Research Facility. A high-temperature flow reactor that can accommodate small preforms (1-3 cm diameter) generates conditions under which deposition can be observed, with flexibility to vary both deposition temperature (up to 1500 K) and pressure (as low as 10 torr). Both mass spectrometric and laser diagnostic probes are available to provide measurements of gas-phase compositions. Experiments using surface analytical techniques are also applied to characterize important processes occuring on the deposit surface. Computational tools developed through extensive research in the combustion field are employed to simulate the chemically reacting flows present in typical industrial reactors. These include the CHEMKIN and Surface-CHEMKIN suites of codes, which permit facile development of complex reaction mechanisms and vastly simplify the implementation of multi-component transport and thermodynamics. Quantum chemistry codes are also used to estimate thermodynamic and kinetic data for species and reactions for which this information is unavailable.

  14. trans-2-Tritylcyclohexanol as a chiral auxiliary in permanganate-mediated oxidative cyclization of 2-methylenehept-5-enoates: application to the synthesis of trans-(+)-linalool oxide.

    Science.gov (United States)

    Al Hazmi, Ali M; Sheikh, Nadeem S; Bataille, Carole J R; Al-Hadedi, Azzam A M; Watkin, Sam V; Luker, Tim J; Camp, Nicholas P; Brown, Richard C D

    2014-10-03

    The permanganate-mediated oxidative cyclization of a series of 2-methylenehept-5-eneoates bearing different chiral auxiliaries was investigated, leading to the discovery of trans-2-tritylcyclohexanol (TTC) as a highly effective chiral controller for the formation of the 2,5-substituted THF diol product with high diastereoselectivity (dr ∼97:3). Chiral resolution of (±)-TTC, prepared in one step from cyclohexene oxide, afforded (-)-(1S,2R)-TTC (er >99:1), which was applied to the synthesis of (+)-trans-(2S,5S)-linalool oxide.

  15. Effect of uridine protecting groups on the diastereoselectivity of uridine-derived aldehyde 5’-alkynylation

    Directory of Open Access Journals (Sweden)

    Raja Ben Othman

    2017-08-01

    Full Text Available The 5’-alkynylation of uridine-derived aldehydes is described. The addition of alkynyl Grignard reagents on the carbonyl group is significantly influenced by the 2’,3’-di-O-protecting groups (R1: O-alkyl groups led to modest diastereoselectivities (65:35 in favor of the 5’R-isomer, whereas O-silyl groups promoted higher diastereoselectivities (up to 99:1 in favor of the 5’S-isomer. A study related to this protecting group effect on the diastereoselectivity is reported.

  16. An Improved, Highly Efficient Method for the Synthesis of Bisphenols

    Directory of Open Access Journals (Sweden)

    L. S. Patil

    2011-01-01

    Full Text Available An efficient synthesis of bisphenols is described by condensation of substituted phenols with corresponding cyclic ketones in presence of cetyltrimethylammonium chloride and 3-mercaptopropionic acid as a catalyst in extremely high purity and yields.

  17. Nanocrystalline Ni-Co Alloy Synthesis by High Speed Electrodeposition

    OpenAIRE

    Idris, Jamaliah; Christian, Chukwuekezie; Gaius, Eyu

    2013-01-01

    Electrodeposition of nanocrystals is economically and technologically viable production path for the synthesis of pure metals and alloys both in coatings and bulk form. The study presents nanocrystalline Ni-Co alloy synthesis by high speed electrodeposition. Nanocrystalline Ni-Co alloys coatings were prepared by direct current (DC) and deposited directly on steel and aluminum substrates without any pretreatment, using high speed electrodeposition method. The influence of the electrolysis par...

  18. An efficient method for synthesis of succinate-based MMP inhibitors.

    Science.gov (United States)

    Sibi, Mukund P; Hasegawa, Hikaru

    2002-10-03

    A differentially protected fumarate undergoes radical addition followed by allylstannane trapping to provide disubstituted succinates in good yields and high anti diastereoselectivity. The conversion of the succinate to a known MMP inhibitor has been accomplished. [reaction: see text

  19. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    OpenAIRE

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-01-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtain...

  20. Stereoselective Catalytic Synthesis of Active Pharmaceutical Ingredients in Homemade 3D-Printed Mesoreactors.

    Science.gov (United States)

    Rossi, Sergio; Porta, Riccardo; Brenna, Davide; Puglisi, Alessandra; Benaglia, Maurizio

    2017-04-03

    3D-printed flow reactors were designed, fabricated from different materials (PLA, HIPS, nylon), and used for a catalytic stereoselective Henry reaction. The use of readily prepared and tunable 3D-printed reactors enabled the rapid screening of devices with different sizes, shapes, and channel dimensions, aimed at the identification of the best-performing reactor setup. The optimized process afforded the products in high yields, moderate diastereoselectivity, and up to 90 % ee. The method was applied to the continuous-flow synthesis of biologically active chiral 1,2-amino alcohols (norephedrine, metaraminol, and methoxamine) through a two-step sequence combining the nitroaldol reaction with a hydrogenation. To highlight potential industrial applications of this method, a multistep continuous synthesis of norephedrine has been realized. The product was isolated without any intermediate purifications or solvent switches. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Concise Stereocontrolled Formal Synthesis of (±)-Quinine and Total Synthesis of (±)-7-Hydroxyquinine via Merged Morita-Baylis-Hillman-Tsuji-Trost Cyclization

    Science.gov (United States)

    Webber, Peter; Krische, Michael J.

    2010-01-01

    Concise stereoselective syntheses of (±)-quinine and (±)-7-hydroxyquinine are achieved using a catalytic enone cycloallylation that combines the nucleophilic features of the Morita-Baylis-Hillman reaction and the electrophilic features of the Tsuji-Trost reaction. Cyclization of enone-allyl carbonate 11 delivers the product of cycloallylation 13 in 68% yield. Diastereoselective conjugate reduction of the enone 13 (>20:1 dr) followed by exchange of N-protecting groups provides the saturated N-Boc-protected methyl ketone 19, which upon aldol dehydration provides quinoline containing enone 15, possessing all carbon atoms of quinine. Exposure of ketone 15 to L-selectride enables diastereoselective carbonyl reduction (>20:1 dr) to furnish the allylic alcohol 16. Stereoselective hydroxyl-directed epoxidation using an oxovanadium catalyst modified by N-hydroxy-N-Me-pivalamide delivers epoxide 17 (17:1 dr). Cyclization of the resulting amine-epoxide 17 provides (±)-7-hydroxyquinine in 13 steps and 11% overall yield from aminoacetaldehyde diethyl acetal. Notably, highly stereoselective formation of five contiguous stereocenters is achieved through a series of 1,2-asymmetric induction events. A formal synthesis of (±)-quinine is achieved upon deoxygenation of the N-Cbz-protected allylic acetate 22 to provide olefin 23, which previously has been converted to quinine. Thus, (±)-quinine is accessible in 16 steps and 4% overall yield from commercial aminoacetaldehyde diethyl acetal, making this route the most concise approach to quinine, to date. PMID:18989927

  2. Regio- and stereoselective 1,2-dihydropyridine alkylation/addition sequence for the synthesis of piperidines with quaternary centers.

    Science.gov (United States)

    Duttwyler, Simon; Chen, Shuming; Lu, Colin; Mercado, Brandon Q; Bergman, Robert G; Ellman, Jonathan A

    2014-04-07

    The first example of C alkylation of 1,2-dihydropyridines with alkyl triflates and Michael acceptors was developed to introduce quaternary carbon centers with high regio- and diastereoselectivity. Hydride or carbon nucleophile addition to the resultant iminium ion also proceeded with high diastereoselectivity. Carbon nucleophile addition results in an unprecedented level of substitution to provide piperidine rings with adjacent tetrasubstituted carbon atoms. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Self-propagating high temperature synthesis and magnetic

    Indian Academy of Sciences (India)

    Ni–Zn ferrite powders were synthesized by self-propagating high temperature synthesis (SHS) method. X-ray diffraction, TEM and vibrating sample magnetometry (VSM) were used to characterize the phase composition, microstructure and magnetic properties of the combustion products. The effect of the combustion ...

  4. Synthesis and spectroscopic study of high quality alloy Cdx S ...

    Indian Academy of Sciences (India)

    Wintec

    In the present study, we report the synthesis of high quality CdxZn1–xS nanocrystals alloy at. 150°C with .... (XRD) using a Siemens model D 500, powder X-ray ... decays were analysed using IBH DAS6 software. 3. ... This alloying process is.

  5. High Friction Surface Treatments, Transportation Research Synthesis

    Science.gov (United States)

    2018-03-01

    MnDOT and local transportation agencies in Minnesota are considering the use of a high friction surface treatment (HFST) as a safety strategy. HFST is used as a spot pavement surfacing treatment in locations with high friction demand (for example, cr...

  6. High pressure synthesis of bismuth disulfide

    DEFF Research Database (Denmark)

    Søndergaard-Pedersen, Simone; Nielsen, Morten Bormann; Bremholm, Martin

    In this research the BiS2 compound was synthesized by a high pressure and high temperature method using a multi-anvil large volume press and the structure was solved by single crystal diffraction. The structure contains Bi atoms in distorted square-based pyramidal coordination to five surrounding...

  7. Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides; Diastereosseletividade na reducao de enonas biciclicas com hidretos volumosos

    Energy Technology Data Exchange (ETDEWEB)

    Camozzato, Andreza C.; Tenius, Beatriz S. M.; Oliveira, Eduardo R. de [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Inst. de Quimica. Dept. de Quimica Organica]. E-mail: eroliv@iq.ufrgs.br; Viegas Junior, Claudio [Universidade Federal de Alfenas (UFAL), MG (Brazil). Dept. de Farmacia; Victor, Mauricio M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica. Dept. de Quimica Organica; Silveira, Leandro G. da [Universidade Regional Integrada do Alto Uruguai e das Missoes, Frederico Westphalen, RS (Brazil). Curso de Quimica. Dept. de Ciencias Exatas e da Terra

    2008-07-01

    Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride{sup R}) in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring. (author)

  8. Diastereoselective Addition of α-Metalated Sulfoxides to Imines Revisited: Mechanism, Computational Studies, and the Effect of External Chiral Ligands

    DEFF Research Database (Denmark)

    Pedersen, Brian; Rein, Tobias; Søtofte, Inger

    2003-01-01

    six-membered "flat chair") was probed by quantum mechanical calculations, which underpinned the idea of using external chiral ligands to enhance the diastereoselectivity of otherwise moderately selective reactions. In this way, the diastereomeric ratio of the product 3a could be raised from (84 : 16...

  9. Total synthesis of the proposed structure of trichodermatide A.

    Science.gov (United States)

    Myers, Eddie; Herrero-Gómez, Elena; Albrecht, Irina; Lachs, Jennifer; Mayer, Peter; Hanni, Matti; Ochsenfeld, Christian; Trauner, Dirk

    2014-10-17

    A short total synthesis of the published structure of racemic trichodermatide A is reported. Our synthesis involves a Knoevenagel condensation/Michael addition sequence, followed by the formation of tricyclic hexahydroxanthene-dione and a diastereoselective bis-hydroxylation. The final product, the structure of which was confirmed by X-ray crystallography, has NMR spectra that are very similar, but not identical, to those of the isolated natural product. Quantum chemically computed (13)C shifts agree well with the present NMR measurements.

  10. Nitrile ylides: diastereoselective cycloadditions using chiral oxazolidinones without Lewis acid.

    Science.gov (United States)

    Sibi, Mukund P; Soeta, Takahiro; Jasperse, Craig P

    2009-12-03

    Lewis acid complexation is generally required for chiral-auxiliary-controlled stereoselectivity, and chiral Lewis acid catalysis is frequently optimal for introducing asymmetry. In this work, we show that nitrile ylide cycloadditions to electron-poor acceptors attached to chiral auxiliaries proceed in high yield and stereoselectivity in the absence of Lewis acids. In contrast, chiral Lewis acids are inferior in these cycloadditions.

  11. Synthesis and Characterization of High Energy Polymers.

    Science.gov (United States)

    1981-03-31

    and characterization of new high energy elastomers. IV. References 1. J.C.W. Chien, T. Kohara , C. P. Lillya, T. Sarubbi, B.-H. Su and R. S. Miller, J...Catalyzed Nitromercuration of Diene Polymers, J.C.W. Chien, T. Kohara , C. P. Lillya, T. Sarubbi, B.-H. Su, and R. S. Miller, J. Polm.. Sci. Polym. Chem. Ed

  12. A concise enantioselective synthesis of the guaiane sesquiterpene (−-oxyphyllol

    Directory of Open Access Journals (Sweden)

    Martin Zahel

    2013-10-01

    Full Text Available (−-Oxyphyllol was prepared in only 4 steps from an epoxy enone that already served as an intermediate for the total synthesis of the anticancer guaiane (−-englerin A. A regio- and diastereoselective Co(II-catalyzed hydration of the olefin and a transannular epoxide opening were used as the key reactions.

  13. (S)-1-Aminoindane : synthesis by chirality transfer using (R)-phenylglycine amide as chiral auxiliary

    NARCIS (Netherlands)

    Uiterweerd, Patrick G.H.; Sluis, Marcel van der; Kaptein, Bernard; Lange, Ben de; Kellogg, Richard M.; Broxterman, Quirinus B.

    2003-01-01

    A practical asymmetric synthesis of nearly enantiomerically pure (S)-1-aminoindane has been developed. The key step involves the diastereoselective heterogeneous metal-catalyzed reduction of the ketimine of 1-indanone with the chiral auxiliary (R)-phenylglycine amide. The selectivity of the

  14. HIGH EFFICIENCY DESULFURIZATION OF SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Anirban Mukherjee; Kwang-Bok Yi; Elizabeth J. Podlaha; Douglas P. Harrison

    2001-11-01

    Mixed metal oxides containing CeO{sub 2} and ZrO{sub 2} are being studied as high temperature desulfurization sorbents capable of achieving the DOE Vision 21 target of 1 ppmv of less H{sub 2}S. The research is justified by recent results in this laboratory that showed that reduced CeO{sub 2}, designated CeO{sub n} (1.5 < n < 2.0), is capable of achieving the 1 ppmv target in highly reducing gas atmospheres. The addition of ZrO{sub 2} has improved the performance of oxidation catalysts and three-way automotive catalysts containing CeO{sub 2}, and should have similar beneficial effects on CeO{sub 2} desulfurization sorbents. An electrochemical method for synthesizing CeO{sub 2}-ZrO{sub 2} has been developed and the products have been characterized by XRD and TEM during year 01. Nanocrystalline particles having a diameter of about 5 nm and containing from approximately 10 mol% to 80 mol% ZrO{sub 2} have been prepared. XRD showed the product to be a solid solution at low ZrO{sub 2} contents with a separate ZrO{sub 2} phase emerging at higher ZrO{sub 2} levels. Phase separation did not occur when the solid solutions were heat treated at 700 C. A flow reactor system constructed of quartz and teflon has been constructed, and a gas chromatograph equipped with a pulsed flame photometric detector (PFPD) suitable for measuring sub-ppmv levels of H{sub 2}S has been purchased with LSU matching funds. Preliminary desulfurization tests using commercial CeO{sub 2} and CeO{sub 2}-ZrO{sub 2} in highly reducing gas compositions has confirmed that CeO{sub 2}-ZrO{sub 2} is more effective than CeO{sub 2} in removing H{sub 2}S. At 700 C the product H{sub 2}S concentration using CeO{sub 2}-ZrO{sub 2} sorbent was near the 0.1 ppmv PFPD detection limit during the prebreakthrough period.

  15. Method for synthesis of high quality graphene

    Science.gov (United States)

    Lanzara, Alessandra [Piedmont, CA; Schmid, Andreas K [Berkeley, CA; Yu, Xiaozhu [Berkeley, CA; Hwang, Choonkyu [Albany, CA; Kohl, Annemarie [Beneditkbeuern, DE; Jozwiak, Chris M [Oakland, CA

    2012-03-27

    A method is described herein for the providing of high quality graphene layers on silicon carbide wafers in a thermal process. With two wafers facing each other in close proximity, in a first vacuum heating stage, while maintained at a vacuum of around 10.sup.-6 Torr, the wafer temperature is raised to about 1500.degree. C., whereby silicon evaporates from the wafer leaving a carbon rich surface, the evaporated silicon trapped in the gap between the wafers, such that the higher vapor pressure of silicon above each of the wafers suppresses further silicon evaporation. As the temperature of the wafers is raised to about 1530.degree. C. or more, the carbon atoms self assemble themselves into graphene.

  16. HIGH EFFICIENCY DESULFURIZATION OF SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Kwang-Bok Yi; Anirban Mukherjee; Elizabeth J. Podlaha; Douglas P. Harrison

    2004-03-01

    Mixed metal oxides containing ceria and zirconia have been studied as high temperature desulfurization sorbents with the objective of achieving the DOE Vision 21 target of 1 ppmv or less H{sub 2}S in the product gas. The research was justified by recent results in this laboratory that showed that reduced CeO{sub 2}, designated CeOn (1.5 < n < 2.0), is capable of achieving the 1 ppmv target in highly reducing gas atmospheres. The addition of ZrO{sub 2} has improved the performance of oxidation catalysts and three-way automotive catalysts containing CeO{sub 2}, and was postulated to have similar beneficial effects on CeO{sub 2} desulfurization sorbents. An electrochemical method for synthesizing CeO{sub 2}-ZrO{sub 2} mixtures was developed and the products were characterized by XRD and TEM during year 01. Nanocrystalline particles having a diameter of about 5 nm and containing from approximately 10 mol% to 80 mol% ZrO{sub 2} were prepared. XRD analysis showed the product to be a solid solution at low ZrO{sub 2} contents with a separate ZrO{sub 2} phase emerging at higher ZrO{sub 2} levels. Unfortunately, the quantity of CeO{sub 2}-ZrO{sub 2} that could be prepared electrochemically was too small to permit desulfurization testing. Also during year 01 a laboratory-scale fixed-bed reactor was constructed for desulfurization testing. All components of the reactor and analytical systems that were exposed to low concentrations of H{sub 2}S were constructed of quartz, Teflon, or silcosteel. Reactor product gas composition as a function of time was determined using a Varian 3800 gas chromatograph equipped with a pulsed flame photometric detector (PFPD) for measuring low H{sub 2}S concentrations from approximately 0.1 to 10 ppmv, and a thermal conductivity detector (TCD) for higher concentrations of H{sub 2}S. Larger quantities of CeO{sub 2}-ZrO{sub 2} mixtures from other sources, including mixtures prepared in this laboratory using a coprecipitation procedure, were obtained

  17. Nanocrystalline Ni-Co Alloy Synthesis by High Speed Electrodeposition

    Directory of Open Access Journals (Sweden)

    Jamaliah Idris

    2013-01-01

    Full Text Available Electrodeposition of nanocrystals is economically and technologically viable production path for the synthesis of pure metals and alloys both in coatings and bulk form. The study presents nanocrystalline Ni-Co alloy synthesis by high speed electrodeposition. Nanocrystalline Ni-Co alloys coatings were prepared by direct current (DC and deposited directly on steel and aluminum substrates without any pretreatment, using high speed electrodeposition method. The influence of the electrolysis parameters, such as cathodic current density and temperature at constant pH, on electrodeposition and microstructure of Ni-Co alloys were examined. A homogeneous surface morphology was obtained at all current densities of the plated samples, and it was evident that the current density and temperature affect the coating thickness of Ni-Co alloy coatings.

  18. High-throughput synthesis equipment applied to polymer research

    NARCIS (Netherlands)

    Hoogenboom, R.; Schubert, U.S.

    2005-01-01

    To speed up synthetic polymer research, a workflow dedicated to automated polymer synthesis and characterization was developed. The workflow consists of several synthesis robots with online and offline analytical equipment. For screening of reaction parameters and for library synthesis, robots

  19. Synthesis of high specific activity tritium labelled compounds

    International Nuclear Information System (INIS)

    Parent, P.

    1986-01-01

    Tritiated methyl iodide of high specific activity is synthetized by Fischer-Tropsch reaction of tritium with carbon monoxide, tritiated methanol obtained is reacted with hydriodic acid. It is used for the synthesis of S-adenosyl L-methionine 3 H-methyl and of diazepam 3 H-methyl derivatives. Synthesis of 3-PPP 3 H: (hydroxy-3 phenyl)-3N-n propyl [ 3 H-2.3] piperidine [ 3 H-2.3] with a specific activity of 4.25 T Bq/mM (115 Ci/mM) and of baclofene 3 H with a specific activity of 0.925 TBq (25 Ci/mM) are also described [fr

  20. Alcohol synthesis in a high-temperature slurry reactor

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, G.W.; Marquez, M.A.; McCutchen, M.S. [North Carolina State Univ., Raleigh, NC (United States)

    1995-12-31

    The overall objective of this contract is to develop improved process and catalyst technology for producing higher alcohols from synthesis gas or its derivatives. Recent research has been focused on developing a slurry reactor that can operate at temperatures up to about 400{degrees}C and on evaluating the so-called {open_quotes}high pressure{close_quotes} methanol synthesis catalyst using this reactor. A laboratory stirred autoclave reactor has been developed that is capable of operating at temperatures up to 400{degrees}C and pressures of at least 170 atm. The overhead system on the reactor is designed so that the temperature of the gas leaving the system can be closely controlled. An external liquid-level detector is installed on the gas/liquid separator and a pump is used to return condensed slurry liquid from the separator to the reactor. In order to ensure that gas/liquid mass transfer does not influence the observed reaction rate, it was necessary to feed the synthesis gas below the level of the agitator. The performance of a commercial {open_quotes}high pressure {close_quotes} methanol synthesis catalyst, the so-called {open_quotes}zinc chromite{close_quotes} catalyst, has been characterized over a range of temperature from 275 to 400{degrees}C, a range of pressure from 70 to 170 atm., a range of H{sub 2}/CO ratios from 0.5 to 2.0 and a range of space velocities from 2500 to 10,000 sL/kg.(catalyst),hr. Towards the lower end of the temperature range, methanol was the only significant product.

  1. Shock-induced synthesis of high temperature superconducting materials

    Science.gov (United States)

    Ginley, D.S.; Graham, R.A.; Morosin, B.; Venturini, E.L.

    1987-06-18

    It has now been determined that the unique features of the high pressure shock method, especially the shock-induced chemical synthesis technique, are fully applicable to high temperature superconducting materials. Extraordinarily high yields are achievable in accordance with this invention, e.g., generally in the range from about 20% to about 99%, often in the range from about 50% to about 90%, lower and higher yields, of course, also being possible. The method of this invention involves the application of a controlled high pressure shock compression pulse which can be produced in any conventional manner, e.g., by detonation of a high explosive material, the impact of a high speed projectile or the effect of intense pulsed radiation sources such as lasers or electron beams. Examples and a discussion are presented.

  2. Build/Couple/Pair and Multifunctional Catalysis Strategies for the Synthesis of Heterocycles from Simple Starting Materials

    DEFF Research Database (Denmark)

    Ascic, Erhad

    . Multifunctional Catalysis: Synthesis of Heterocycles from Simple Starting Materials A multifunctional catalysis approach, involving a ruthenium-catalyzed tandem ringclosing metathesis/isomerization/N-acyliminium cyclization sequence, is described. Double bonds created during ring-closing metathesis isomerize......, a series of interesting indolizidinones are formed in good yields with excellent diastereoselectivities, including a formal total synthesis of the antiparasitic natural product harmicine and the first total synthesis of mescalotam. Furthermore, preliminary asymmetric variants of the tandem process have...

  3. Synthesis of (±)-amathaspiramide F and discovery of an unusual stereocontrolling element for the [2,3]-Stevens rearrangement.

    Science.gov (United States)

    Soheili, Arash; Tambar, Uttam K

    2013-10-04

    A formal total synthesis of (±)-amathaspiramide F through a tandem palladium-catalyzed allylic amination/[2,3]-Stevens rearrangement is reported. The unexpected diastereoselectivity of the [2,3]-Stevens rearrangement was controlled by the substitution patterns of an aromatic ring. This discovery represents a new stereocontrolling element for [2,3]-sigmatropic rearrangements in complex molecular settings.

  4. Studies on synthesis of diamond at high pressure and temperature

    Science.gov (United States)

    Kailath, Ansu J.

    Diamond is an essential material of modern industry and probably the most versatile abrasive available today. It also has many other industrial applications attributable to its unique mechanical, optical, thermal and electrical properties. Its usage has grown to the extent that there is hardly a production process in modern industry in which industrial diamond does not play a part. Bulk diamond production today is a major industry. Diamonds can be produced in its thermodynamically stable regions either by direct static conversion, or shock-wave conversion. The pressures and temperatures required for direct static conversion are very high. In the catalyst-solvent method, the material used establishes a reaction path with lower activation energy than for direct transformation. This helps in a quicker transformation under more benign conditions. Hence, catalyst-solvent synthesis is readily accomplished and is now a viable and successful industrial process. Diamonds produced by shock wave are very small (approximately 60mu). Therefore this diamond is limited to applications such as polishing compounds only. The quality, quantity, size and morphology of the crystals synthesized by catalyst-solvent process depend on different conditions employed for synthesis. These details, because of commercial reasons are not disclosed in published literature. Hence, systematic studies have been planned to investigate the effect of various growth parameters on the synthesized crystals. During the growth of synthetic diamond crystals, some catalyst-solvent is retained into the crystals in some form and behaves like an impurity. Several physico-mechanical properties of the crystals are found to depend on the total quantity and distribution of these inclusions. Thus, detailed investigation of the crystallization medium and inclusions in synthesized diamonds was also undertaken in the present work. The work incorporated in this thesis has been divided into seven chapters. The first

  5. A stereoselective, catalytic strategy for the in-flow synthesis of advanced precursors of rasagiline and tamsulosin.

    Science.gov (United States)

    Brenna, Davide; Pirola, Margherita; Raimondi, Laura; Burke, Anthony J; Benaglia, Maurizio

    2017-12-01

    The diastereoselective, trichlorosilane-mediate reduction of imines, bearing different and removable chiral auxiliaries, in combination either with achiral bases or catalytic amounts of chiral Lewis bases, was investigated to afford immediate precursors of chiral APIs (Active Pharmaceutical Ingredients). The carbon-nitrogen double bond reduction was successfully performed in batch and in flow mode, in high yields and almost complete stereocontrol. By this metal-free approach, the formal synthesis of rasagiline and tamsulosin was successfully accomplished in micro(meso) flow reactors, under continuous flow conditions. The results of these explorative studies represent a new, important step towards the development of automated processes for the preparation of enantiopure biologically active compounds. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Studies Toward the Asymmetric Synthesis of the Right Part of the Mycalamides

    OpenAIRE

    Zhong, H. Marlon; Sohn, Jeong-Hun; Rawal, Viresh H.

    2007-01-01

    Described herein is the asymmetric synthesis of a functionalized, trioxadecalin unit that comprises the right-hand part of the mycalamides and related natural products. The synthetic route involves a 16-step sequence that accomplishes the formation of two heterocyclic rings and the generation of five stereocenters. The synthesis commenced with a C2 symmetric starting material, diethyl D-tartrate, and took advantage of a relay of diastereoselective reactions to extend this four-carbon chain an...

  7. The Brønsted Acid-Catalyzed, Enantioselective Aza-Diels-Alder Reaction for the Direct Synthesis of Chiral Piperidones.

    Science.gov (United States)

    Weilbeer, Claudia; Sickert, Marcel; Naumov, Sergei; Schneider, Christoph

    2017-01-12

    We disclose herein the first enantioselective aza-Diels-Alder reaction of β-alkyl-substituted vinylketene silyl-O,O-acetals and imines furnishing a broad range of optically highly enriched 4-alkyl-substituted 2-piperidones. As a catalyst for this one-pot reaction we employed a chiral phosphoric acid which effects a vinylogous Mannich reaction directly followed by ring-closure to the lactam. Subsequent fully diastereoselective transformations including hydrogenation, enolate alkylation, and lactam alkylation/reduction processes converted the cycloadducts into various highly substituted piperidines of great utility for the synthesis of natural products and medicinally active compounds. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. High temperature bismuth cuprate superconductors synthesis and characterization

    International Nuclear Information System (INIS)

    Mansori, M.; Satre, P.; Breandon, C.; Roubin, M.; Sebaoun, A.

    1993-01-01

    High temperature superconductor phases synthesis by coprecipitation in alkaline solution is reported. (Bi 1.6 Pb 0.4 )Sr 2 Ca 1 Cu 2 O 8+x and (Bi 1.6 Pb 0.4 )Sr 2 Ca 2 Cu 3 O 10+y noted (2212) and (2223) have been prepared and studied. From aqueous nitrate solutions of Bi, Pb, Sr, Ca and Cu and oxalic acid aqueous solution as well as ethylene glycol, using an organic base (the triethylamine), the pH was increased up to the path of the precipitation zone (pH = 10.5-11.2). This method assures a good granulometric homogeneity of powders. Thermal analysis and characterization of the different components produced during the synthesis have been studied by DTA (differential thermal analysis)- TGA (thermogravimetric analysis), X-ray diffraction at different temperatures and by Infrared spectroscopy with a Fourier transformation. The measurements of magnetic susceptibility for the 2212 (with and without lead) and 2223 (with lead) phases have permitted us to observe the critical temperatures of 84 K, 87 K and 114 K. (author). 29 refs., 2 figs., 4 tabs

  9. Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants.

    Science.gov (United States)

    Wang, Junlian; Xie, Meiying; Liu, Xinyu; Xu, Shengming

    2017-10-19

    We present the synthesis of (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high purity nonsymmetric dialkylphosphinic acid extractants. Low toxic sodium hypophosphite was chosen as the phosphorus source to react with olefin A (2,3-dimethyl-1-butene) to generate a monoalkylphosphinic acid intermediate. Amantadine was adopted to remove the dialkylphosphinic acid byproduct, as only the monoalkylphosphinic acid can react with amantadine to form an amantadine∙mono-alkylphosphinic acid salt, while the dialkylphosphinic acid cannot react with amantadine due to its large steric hindrance. The purified monoalkylphosphinic acid was then reacted with olefin B (diisobutylene) to yield nonsymmetric dialkylphosphinic acid (NSDAPA). The unreacted monoalkylphosphinic acid can be easily removed by a simple base-acid post-treatment and other organic impurities can be separated out through the precipitation of the cobalt salt. The structure of the (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid was confirmed by 31 P NMR, 1 H NMR, ESI-MS, and FT-IR. The purity was determined by a potentiometric titration method, and the results indicate that the purity can exceed 96%.

  10. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-03-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

  11. Multiple Word-Length High-Level Synthesis

    Directory of Open Access Journals (Sweden)

    Coussy Philippe

    2008-01-01

    Full Text Available Abstract Digital signal processing (DSP applications are nowadays widely used and their complexity is ever growing. The design of dedicated hardware accelerators is thus still needed in system-on-chip and embedded systems. Realistic hardware implementation requires first to convert the floating-point data of the initial specification into arbitrary length data (finite-precision while keeping an acceptable computation accuracy. Next, an optimized hardware architecture has to be designed. Considering uniform bit-width specification allows to use traditional automated design flow. However, it leads to oversized design. On the other hand, considering non uniform bit-width specification allows to get a smaller circuit but requires complex design tasks. In this paper, we propose an approach that inputs a C/C++ specification. The design flow, based on high-level synthesis (HLS techniques, automatically generates a potentially pipeline RTL architecture described in VHDL. Both bitaccurate integer and fixed-point data types can be used in the input specification. The generated architecture uses components (operator, register, etc. that have different widths. The design constraints are the clock period and the throughput of the application. The proposed approach considers data word-length information in all the synthesis steps by using dedicated algorithms. We show in this paper the effectiveness of the proposed approach through several design experiments in the DSP domain.

  12. Multiple Word-Length High-Level Synthesis

    Directory of Open Access Journals (Sweden)

    Dominique Heller

    2008-09-01

    Full Text Available Digital signal processing (DSP applications are nowadays widely used and their complexity is ever growing. The design of dedicated hardware accelerators is thus still needed in system-on-chip and embedded systems. Realistic hardware implementation requires first to convert the floating-point data of the initial specification into arbitrary length data (finite-precision while keeping an acceptable computation accuracy. Next, an optimized hardware architecture has to be designed. Considering uniform bit-width specification allows to use traditional automated design flow. However, it leads to oversized design. On the other hand, considering non uniform bit-width specification allows to get a smaller circuit but requires complex design tasks. In this paper, we propose an approach that inputs a C/C++ specification. The design flow, based on high-level synthesis (HLS techniques, automatically generates a potentially pipeline RTL architecture described in VHDL. Both bitaccurate integer and fixed-point data types can be used in the input specification. The generated architecture uses components (operator, register, etc. that have different widths. The design constraints are the clock period and the throughput of the application. The proposed approach considers data word-length information in all the synthesis steps by using dedicated algorithms. We show in this paper the effectiveness of the proposed approach through several design experiments in the DSP domain.

  13. Synthesis of titanium carbide from wood by self-propagating high temperature synthesis

    Directory of Open Access Journals (Sweden)

    Sutham Niyomwas

    2010-05-01

    Full Text Available Titanium carbide (TiC particles were obtained in situ by a self-propagating high temperature synthesis (SHS of wooddust with TiO2 and Mg. The reaction was carried out in a SHS reactor under static argon gas at the pressure of 0.5 MPa. Thestandard Gibbs energy minimization method was used to calculate the equilibrium composition of the reacting species. Theeffects of increasing Mg mole ratio to the precursor mixture of TiO2 and wood dusts were investigated. XRD and SEManalyses indicate a complete reaction of the precursors to yield TiC-MgO as a product composite. The synthesized compositeswere leached with 0.1M HCl acid solution to obtain TiC particles as final products.

  14. A divergent [5+2] cascade approach to bicyclo[3.2.1]octanes: facile synthesis of ent-kaurene and cedrene-type skeletons.

    Science.gov (United States)

    He, Chi; Bai, Zengbing; Hu, Jialei; Wang, Bingnan; Xie, Hujun; Yu, Lei; Ding, Hanfeng

    2017-07-25

    A solvent-dependent oxidative dearomatization-induced divergent [5+2] cascade approach to bicyclo[3.2.1]octanes was described. This novel protocol enables a facile synthesis of a series of diversely functionalized ent-kaurene and cedrene-type skeletons in good yields and excellent diastereoselectivities.

  15. Combinatorial chemoenzymatic synthesis and high-throughput screening of sialosides.

    Science.gov (United States)

    Chokhawala, Harshal A; Huang, Shengshu; Lau, Kam; Yu, Hai; Cheng, Jiansong; Thon, Vireak; Hurtado-Ziola, Nancy; Guerrero, Juan A; Varki, Ajit; Chen, Xi

    2008-09-19

    Although the vital roles of structures containing sialic acid in biomolecular recognition are well documented, limited information is available on how sialic acid structural modifications, sialyl linkages, and the underlying glycan structures affect the binding or the activity of sialic acid-recognizing proteins and related downstream biological processes. A novel combinatorial chemoenzymatic method has been developed for the highly efficient synthesis of biotinylated sialosides containing different sialic acid structures and different underlying glycans in 96-well plates from biotinylated sialyltransferase acceptors and sialic acid precursors. By transferring the reaction mixtures to NeutrAvidin-coated plates and assaying for the yields of enzymatic reactions using lectins recognizing sialyltransferase acceptors but not the sialylated products, the biotinylated sialoside products can be directly used, without purification, for high-throughput screening to quickly identify the ligand specificity of sialic acid-binding proteins. For a proof-of-principle experiment, 72 biotinylated alpha2,6-linked sialosides were synthesized in 96-well plates from 4 biotinylated sialyltransferase acceptors and 18 sialic acid precursors using a one-pot three-enzyme system. High-throughput screening assays performed in NeutrAvidin-coated microtiter plates show that whereas Sambucus nigra Lectin binds to alpha2,6-linked sialosides with high promiscuity, human Siglec-2 (CD22) is highly selective for a number of sialic acid structures and the underlying glycans in its sialoside ligands.

  16. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    Science.gov (United States)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  17. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

    2013-06-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

  18. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    International Nuclear Information System (INIS)

    Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

    2013-01-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

  19. Highly Selective Synthesis of Catalytically Active Monodisperse Rhodium Nanocubes

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Y.; Grass, M.E.; Kuhn, J.N.; Tao, F.; Habas, S.E.; Huang, W.; Yang, P.; Somorjai, G.A.

    2009-02-21

    Synthesis of monodisperse and shape-controlled colloidal inorganic nanocrystals (NCs) is of increasing scientific interest and technological significance. Recently, shape control of Pt, Pd, Ag, Au, and Rh NCs has been obtained by tuning growth kinetics in various solution-phase approaches, including modified polyol methods, seeded growth by polyol reduction, thermolysis of organometallics, and micelle techniques. Control of reduction kinetics of the noble metal precursors and regulation of the relative growth rates of low-index planes (i.e. {l_brace}100{r_brace} and {l_brace}111{r_brace}) via selective adsorption of selected chemical species are two keys for achieving shape modification of noble metal NCs. One application for noble metal NCs of well-defined shape is in understanding how NC faceting (determines which crystallographic planes are exposed) affects catalytic performance. Rh NCs are used in many catalytic reactions, including hydrogenation, hydroformylation, hydrocarbonylation, and combustion reactions. Shape manipulation of Rh NCs may be important in understanding how faceting on the nanoscale affects catalytic properties, but such control is challenging and there are fewer reports on the shape control of Rh NCs compared to other noble metals. Xia and coworkers obtained Rh multipods exhibiting interesting surface plasmonic properties by a polyol approach. The Somorjai and Tilley groups synthesized crystalline Rh multipods, cubes, horns and cuboctahedra, via polyol seeded growth. Son and colleagues prepared catalytically active monodisperse oleylamine-capped tetrahedral Rh NCs for the hydrogenation of arenes via an organometallic route. More recently, the Somorjai group synthesized sizetunable monodisperse Rh NCs using a one-step polyol technique. In this Communication, we report the highly selective synthesis of catalytically active, monodisperse Rh nanocubes of < 10 nm by a seedless polyol method. In this approach, Br{sup -} ions from trimethyl

  20. High pressure synthesis of BiS2

    DEFF Research Database (Denmark)

    Søndergaard-Pedersen, Simone; Nielsen, Morten Bormann; Bremholm, Martin

    crystal structures and electrical properties.1,2 Up until now, the most sulfur rich phase in the Bi-S phase diagram was Bi2S3.3 For BiS2 the Bi atoms have anisotropic charge distribution and more complex structures are expected when comparing the layered structures of transition metal dichalcogenides....... The possibilities of using high pressure synthesis to discover new phases in the Bi-S binary system were investigated as early as the 1960’s.4 The research led to discovery of a compound with BiS2 stoichiometry, but no structure solution of BiS2 was reported. A reason behind making this new phase is to study...... the physical properties since the related compound Bi2S3 is known to be a thermoelectric material.5 In this research the BiS2 compound was synthesized by a high pressure and high temperature method using a multi-anvil large volume press and the structure was solved by single crystal diffraction. The structure...

  1. High pressure direct synthesis of adipic acid from cyclohexene and hydrogen peroxide via capillary microreactors

    NARCIS (Netherlands)

    Shang, M.; Noël, T.; Su, Y.; Hessel, V.

    2016-01-01

    The direct synthesis of adipic acid from hydrogen peroxide and cyclohexene was investigated in capillary microreactors at high temperature (up to 115°C ) and pressure (up to 70 bar). High temperature was already applied in micro-flow packed-bed reactors for the direct adipic acid synthesis. In our

  2. Combining multi-catalysis and multi-component systems for the development of one-pot asymmetric reactions: stereoselective synthesis of highly functionalized bicyclo[4.4.0]decane-1,6-diones.

    Science.gov (United States)

    Ramachary, Dhevalapally B; Sakthidevi, Rajasekar

    2008-07-21

    We have developed a direct amine/acid-catalyzed stereoselective hydrogenation of a variety of Wieland-Miescher (W-M) ketones, Hajos-Parrish (H-P) ketones and their analogs with organic hydrides (Hantzsch esters) as the hydrogen source. This astonishingly simple and biomimetic approach was used to construct highly functionalized chiral bicyclo[4.4.0]decane-1,6-diones in a diastereoselective fashion. This is an example of the development of a new technology by the combination of multiple catalysts and components in one pot to deliver highly functionalized chiral molecules.

  3. High pressure and microwave based synthesis of transition metal pnictides

    Energy Technology Data Exchange (ETDEWEB)

    Pobel, Roman Rupert

    2016-04-11

    The goal of this thesis was to explore the possibilities of synthetic methods that are not very common in current transition metal pnictide research. The substitution of the Ca-site in CaFe{sub 2}As{sub 2} with rare earth elements such as Pr the has been reported to induce superconductivity. However, some inconsistencies in the data suggested a non-intrinsic origin of the observed diamagnetic signal. Furthermore a solubility limit of 13% was found when prepared in an electrical furnace thus leaving a huge part of the physical phase diagram inaccessible. A high pressure/high temperature synthesis was developed to allow access to the whole doping range and an in-depth characterization of this compound was carried out. During the experiments concerning the high pressure synthesis of Ca{sub 1-x}Pr{sub x}Fe{sub 2}As{sub 2} the new ternary iron arsenide CaFe{sub 5}As{sub 3} was identified and classified as a member of the Ca{sub n(n+1)/2}(Fe{sub 1-x}M{sub x}){sub (2+3n)}M'{sub n(n-1)/2}As{sub (n+1)(n+2)/2} (n = 1-3; M =Nb, Pd, Pt; M' = □, Pd, Pt) family. The complete solid solution Ca{sub 1-x}Pr{sub x}Fe{sub 5}As{sub 3} (O ≤ x ≤ 1) was prepared and physically characterized. Furthermore, several useful techniques were developed to aid in future high pressure based investigations of transition metal pnictides. The second part of this thesis concerns a completely different, but equally promising synthetic approach. Microwave based synthesis is a well-established technique in many solution based fields, such as organic, medicinal or nano chemistry. For solid state and materials research several parameters and particularities have to be considered. But when successful, it allows for the reduction of reaction time by several orders of magnitude. It has very rarely been applied in the preparation of pnictides and on1y once in the context of pnictide superconductor research. The possibilities of this method were explored and employed in the preparation of several

  4. N-Heterocyclic Carbene-Catalysed Diastereoselective Vinylogous Michael Addition Reaction of gamma-Substituted deconjugated Butenolides

    KAUST Repository

    Guo, Hao; Xing, Fen; Du, Guang-Fen; Huang, Kuo-Wei; Dai, Bin; He, Lin

    2015-01-01

    An efficient N-heterocyclic carbene (NHC)-catalysed vinylogous Michael addition of deconjugated butenolides was developed. In the presence of 5 mol% of the NHC catalyst, both γ-alkyl and aryl-substituted deconjugated butenolides undergo vinylogous Michael addition with various α, β-unsaturated ketones, esters, or nitriles to afford γ,γ-disubstituted butenolides containing adjacent quaternary and tertiary carbon centers in good to excellent yields with excellent diastereoselectivities. In this process, the free carbene is assumed to act as a strong Brønsted base to promote the conjugate addition.

  5. N-Heterocyclic Carbene-Catalysed Diastereoselective Vinylogous Michael Addition Reaction of gamma-Substituted deconjugated Butenolides

    KAUST Repository

    Guo, Hao

    2015-11-16

    An efficient N-heterocyclic carbene (NHC)-catalysed vinylogous Michael addition of deconjugated butenolides was developed. In the presence of 5 mol% of the NHC catalyst, both γ-alkyl and aryl-substituted deconjugated butenolides undergo vinylogous Michael addition with various α, β-unsaturated ketones, esters, or nitriles to afford γ,γ-disubstituted butenolides containing adjacent quaternary and tertiary carbon centers in good to excellent yields with excellent diastereoselectivities. In this process, the free carbene is assumed to act as a strong Brønsted base to promote the conjugate addition.

  6. Synthesis of High-Molecular-Weight Multifunctional Glycerol Polyhydroxyurethanes PHUs

    Directory of Open Access Journals (Sweden)

    Bassam Nohra

    2016-09-01

    Full Text Available Glycerol carbonate acrylate is a 5-membered cyclic carbonate synthesized from glycerol that is used as a chemical coupling agent and has proven highly suitable for use in the synthesis of multifunctional polyhydroxyurethanes (PHUs. The multifunctionality of the structure of PHUs is determined by the density of the carbon-amine groups generated by the Aza-Michael reaction and that of the urethane groups and adjacent primary and secondary hydroxyl groups generated by aminolysis. Glycerol carbonate acrylate is polymerized with polyfunctional mono-, di-, tri, and tetra-amines, by type-AB polyaddition, either in bulk or in solution, through stepwise or one-pot reaction strategies in the absence of added catalysts. These approaches result in the generation of linear, interchain, and crosslinked structures, through the polyaddition of linear and branched amines to the ethylene and cyclic carbonate sites of glycerol carbonate acrylate. The resulting collection of organic molecules gives rise to polyethylene amino ester PHUs with a high molar mass, exceeding 20,000 g·mol−1, with uniform dispersity.

  7. High-Level Synthesis: Productivity, Performance, and Software Constraints

    Directory of Open Access Journals (Sweden)

    Yun Liang

    2012-01-01

    Full Text Available FPGAs are an attractive platform for applications with high computation demand and low energy consumption requirements. However, design effort for FPGA implementations remains high—often an order of magnitude larger than design effort using high-level languages. Instead of this time-consuming process, high-level synthesis (HLS tools generate hardware implementations from algorithm descriptions in languages such as C/C++ and SystemC. Such tools reduce design effort: high-level descriptions are more compact and less error prone. HLS tools promise hardware development abstracted from software designer knowledge of the implementation platform. In this paper, we present an unbiased study of the performance, usability and productivity of HLS using AutoPilot (a state-of-the-art HLS tool. In particular, we first evaluate AutoPilot using the popular embedded benchmark kernels. Then, to evaluate the suitability of HLS on real-world applications, we perform a case study of stereo matching, an active area of computer vision research that uses techniques also common for image denoising, image retrieval, feature matching, and face recognition. Based on our study, we provide insights on current limitations of mapping general-purpose software to hardware using HLS and some future directions for HLS tool development. We also offer several guidelines for hardware-friendly software design. For popular embedded benchmark kernels, the designs produced by HLS achieve 4X to 126X speedup over the software version. The stereo matching algorithms achieve between 3.5X and 67.9X speedup over software (but still less than manual RTL design with a fivefold reduction in design effort versus manual RTL design.

  8. High Throughput Synthesis and Screening for Agents Inhibiting Androgen Receptor Mediated Gene Transcription

    National Research Council Canada - National Science Library

    Boger, Dale L

    2005-01-01

    .... This entails the high throughput synthesis of DNA binding agents related to distamycin, their screening for binding to androgen response elements using a new high throughput DNA binding screen...

  9. High Throughout Synthesis and Screening for Agents Inhibiting Androgen Receptor Mediated Gene Transcription

    National Research Council Canada - National Science Library

    Boger, Dale

    2003-01-01

    .... This entails the high throughput synthesis of DNA binding agents related to distamycin, their screening for binding to androgen response elements using a new high throughput DNA binding screen...

  10. High Throughput Synthesis and Screening for Agents Inhibiting Androgen Receptor Mediated Gene Transcription

    National Research Council Canada - National Science Library

    Boger, Dale

    2004-01-01

    .... This entails the high throughput synthesis of DNA binding agents related to distamycin, their screening for binding to androgen response elements using a new high throughput DNA binding screen...

  11. High-pressure-assisted synthesis of high-volume ZnGeP2 polycrystalline

    Science.gov (United States)

    Huang, Changbao; Wu, Haixin; Xiao, Ruichun; Chen, Shijing; Ma, Jiaren

    2018-06-01

    The pnictide and chalcogenide semiconductors are promising materials for the applications in the field of photoelectric. High-purity and high-volume polycrystalline required in the real-world applications is hard to be synthesized due to the high vapor pressure of phosphorus and sulfur components at high temperature. A new high-pressure-resisted method was used to investigate the synthesis of the nonlinear-optical semiconductor ZnGeP2. The high-purity ZnGeP2 polycrystalline material of approximately 500 g was synthesized in one run, which enables the preparation of nominally stoichiometric material. Since increasing internal pressure resistance of quartz crucible and reducing the reaction space, the high-pressure-resisted method can be used to rapidly synthesize other pnictide and chalcogenide semiconductors and control the components ratio.

  12. An efficient protocol for the synthesis of highly sensitive indole imines utilizing green chemistry: optimization of reaction conditions.

    Science.gov (United States)

    Nisar, Bushra; Rubab, Syeda Laila; Raza, Abdul Rauf; Tariq, Sobia; Sultan, Ayesha; Tahir, Muhammad Nawaz

    2018-04-11

    Novel and highly sensitive indole-based imines have been synthesized. Their synthesis has been compared employing a variety of protocols. Ultimately, a convenient, economical and high yielding set of conditions employing green chemistry have been designed for their synthesis.

  13. High yield polyol synthesis of round- and sharp-end silver nanowires with high aspect ratio

    Energy Technology Data Exchange (ETDEWEB)

    Nekahi, A.; Marashi, S.P.H., E-mail: pmarashi@aut.ac.ir; Fatmesari, D. Haghshenas

    2016-12-01

    Long silver nanowires (average length of 28 μm, average aspect ratio of 130) with uniform diameter along their length were produced by polyol synthesis of AgNO{sub 3} in ethylene glycol in the presence of PVP as preferential growth agent. Nanowires were produced with no addition of chloride salts such as NaCl or CuCl{sub 2} (or other additives such as Na{sub 2}S) which are usually used for lowering reduction rate of Ag ions by additional etchant of O{sub 2}/Cl{sup −}. Lower reduction rate was obtained by increasing the injection time of PVP and AgNO{sub 3} solutions, which was the significant factor in the formation of nanowires. Therefore, there was enough time for reduced Ag atoms to be deposited preferentially in the direction of PVP chains, resulting in high yield (the fraction of nanowires in the products) of nanowires (more than 95%) with high aspect ratio. The produced nanowires had both round- and sharp-ends with pentagonal cross section. Higher energy level of Ag atoms in borders of MTPs, which increases the dissolution rate of precipitated atoms, in addition to partial melting of MTPs at high synthesis temperatures, leads to the curving of the surfaces of exposed (111) crystalline planes in some MTPs and the formation of round-end silver nanowires. - Highlights: • Long silver nanowires with high aspect ratio of 130 were produced. • More than 95% nanowires were produced in products. • The produced nanowires had round- and sharp-ends with pentagonal cross section. • Additives were needed neither for high yield synthesis nor for round-end nanowires. • Melting and etching of MTPs in high energy borders resulted to round-end nanowires.

  14. Synthesis of lanthanum tungstate interconnecting nanoparticles by high voltage electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Keereeta, Yanee, E-mail: ynkeereeta@gmail.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thongtem, Titipun, E-mail: ttpthongtem@yahoo.com [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thongtem, Somchai [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

    2015-10-01

    Graphical abstract: - Highlights: • La{sub 2}(WO{sub 4}){sub 3} as one of semiconducting materials. • H.V. electrospinning was used to synthesize La{sub 2}(WO{sub 4}){sub 3} interconnecting nanoparticles. • A promising material for photoemission. - Abstract: Lanthanum tungstate (La{sub 2}(WO{sub 4}){sub 3}) interconnecting nanoparticles in the shape of fibers were successfully synthesized by electrospinning in combination with high temperature calcination. In this research, calcination temperature for the synthesis of the fibers evidently influenced the diameter, morphology and crystalline degree. The crystalline monoclinic La{sub 2}(WO{sub 4}){sub 3} fibers with 200–700 nm in diameter, two main Raman peaks at 945 and 927 cm{sup −1}, FTIR stretching modes at 936 and 847 cm{sup −1}, 2.02 eV energy gap and 415–430 nm blue emission were synthesized by calcination of inorganic/organic hybrid fibers at 750 °C for 5 h, characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, UV–visible spectroscopy and photoluminescence (PL) spectroscopy. The surface of the composite fibers before calcination was very smooth. Upon calcination the composite fibers at 750 °C for 5 h, they were transformed into nanoparticles join together in the shape of fibers with rough surface.

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

    Indian Academy of Sciences (India)

    and KANIKA VIJ. Department of Chemistry, University of Delhi, Delhi 110 007, India ... Keywords. PVP-stabilized Ni nanoparticles; ethylene glycol; tetraketones; biscoumarins; ... ing interest in using nickel nanoparticles in organic synthesis ...

  16. Self-sustained high-temperature reactions : Initiation, propagation and synthesis

    NARCIS (Netherlands)

    Martinez Pacheco, M.

    2007-01-01

    Self-Propagating High-Temperature Synthesis (SHS), also called combustion synthesis is an exothermic and self-sustained reaction between the constituents, which has assumed significance for the production of ceramics and ceramic-metallic materials (cermets), because it is a very rapid processing

  17. Ammonia synthesis over multi-promoted iron catalysts obtained by high-energy ball-milling

    DEFF Research Database (Denmark)

    Jacobsen, C.J.H.; Jiang, Jianzhong; Mørup, Steen

    1999-01-01

    The feasibility of producing ammonia synthesis catalysts from high-energy ball-milling of a simple mixture of the constituent oxides has been investigated. The effect of ball-milling the fused oxidic precursor of the industrial KM1 ammonia synthesis catalyst has also been studied. The results show...

  18. Highly enantio- and diastereoselective reactions of γ-substituted butenolides through direct vinylogous conjugate additions

    KAUST Repository

    Zhang, Wen; Tan, Davin; Lee, Richmond; Tong, Guanghu; Chen, Wenchao; Qi, Baojian; Huang, Kuo-Wei; Tan, Choonhong; Jiang, Zhiyong

    2012-01-01

    The strength of the weak: An L-tert-leucine-derived amine-thiourea catalyst (see scheme, green box) promotes the asymmetric vinylogous conjugate addition reaction between γ-aryl- and alkyl-substituted butenolides with the butenamides and enoates shown. Computational studies show the preference for the observed stereochemistry is a result of favourable weak non-bonding interactions, which stabilize the transition state. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Highly enantio- and diastereoselective allylic alkylation of Morita-Baylis-Hillman carbonates with allyl ketones

    KAUST Repository

    Tong, Guanghu

    2013-05-17

    The asymmetric allylic alkylation of Morita-Baylis-Hillman (MBH) carbonates with allyl ketones has been developed. The α-regioselective alkylation adducts, containing a hexa-1,5-diene framework with important synthetic value, were achieved in up to 83% yield, >99% ee, and 50:1 dr by using a commercially available Cinchona alkaloid as the catalyst. From the allylic alkylation adduct, a cyclohexene bearing two adjacent chiral centers was readily prepared. © 2013 American Chemical Society.

  20. Highly enantio- and diastereoselective reactions of γ-substituted butenolides through direct vinylogous conjugate additions

    KAUST Repository

    Zhang, Wen

    2012-09-05

    The strength of the weak: An L-tert-leucine-derived amine-thiourea catalyst (see scheme, green box) promotes the asymmetric vinylogous conjugate addition reaction between γ-aryl- and alkyl-substituted butenolides with the butenamides and enoates shown. Computational studies show the preference for the observed stereochemistry is a result of favourable weak non-bonding interactions, which stabilize the transition state. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Highly enantio- and diastereoselective allylic alkylation of Morita-Baylis-Hillman carbonates with allyl ketones

    KAUST Repository

    Tong, Guanghu; Zhu, Bo; Lee, Richmond; Yang, Wenguo; Tan, Davin; Yang, Caiyun; Han, Zhiqiang; Yan, Lin; Huang, Kuo-Wei; Jiang, Zhiyong

    2013-01-01

    The asymmetric allylic alkylation of Morita-Baylis-Hillman (MBH) carbonates with allyl ketones has been developed. The α-regioselective alkylation adducts, containing a hexa-1,5-diene framework with important synthetic value, were achieved in up to 83% yield, >99% ee, and 50:1 dr by using a commercially available Cinchona alkaloid as the catalyst. From the allylic alkylation adduct, a cyclohexene bearing two adjacent chiral centers was readily prepared. © 2013 American Chemical Society.

  2. Diastereosseletividade na redução de enonas bicíclicas com hidretos volumosos Diastereoselectivity in the reduction of bicyclic enones with hindered hydrides

    Directory of Open Access Journals (Sweden)

    Andreza C. Camozzato

    2008-01-01

    Full Text Available Reduction of five substituted octalones employing lithium tri-sec-butylborohydride (L-selectride® in THF and ethyl ether led to allylic alcohols with moderate diastereoselectivity. The stereoselectivity of addition of bulky hydrides showed to be different from most examples in the literature and was strongly influenced by substitution on the octalone ring.

  3. Development of coating technology for nuclear fuel by self-propagating high temperature synthesis

    International Nuclear Information System (INIS)

    Choi, Y.; Kim, Bong G.; Lee, Y. W.

    1997-01-01

    This paper presents experimental results of the preparation of silicon carbide and graphite layers on a nuclear fuel from silane and propane gases by a conventional chemical vapor deposition and combustion synthesis technologies. The direct reaction between silicon and pyrolytic carbon in a high temperature releases sufficient amount of energy to make a synthesis self-sustaining under the preheating of about 1200 deg C. During this high temperature process, lamellar structure with isotropic carbon synthesis. A full characterization of phase composition and final morphology of the coated layers by X-ray diffraction, SEM and AES is presented. (author). 6 refs., 1 tab., 11 figs

  4. Stereoselective synthesis of novel highly substituted isochromanone and isoquinolinone-containing exocyclic tetrasubstituted alkenes.

    Science.gov (United States)

    Arthuis, Martin; Pontikis, Renée; Florent, Jean-Claude

    2009-03-06

    An efficient synthetic route toward the synthesis of highly substituted arylethylidene-isoquinolinones/isochromanones is reported. The tandem carbopalladation/Suzuki-Miyaura coupling sequence stereoselectively provided various functionalized polycyclic compounds in moderate to excellent yields.

  5. Self-propagating high-temperature synthesis of nonstoichiometric wuestite

    Energy Technology Data Exchange (ETDEWEB)

    Hiramoto, Maki [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Okinaka, Noriyuki [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Akiyama, Tomohiro, E-mail: takiyama@eng.hokudai.ac.jp [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan)

    2012-04-15

    Highlights: Black-Right-Pointing-Pointer The manuscript describes an SHS method of producing Fe{sub x}O. Black-Right-Pointing-Pointer Focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. Black-Right-Pointing-Pointer Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Black-Right-Pointing-Pointer Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating. - Abstract: This paper describes the self-propagating high-temperature synthesis (SHS) of nonstoichiometric Fe{sub x}O (x = 0.833-1), with particular focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. In the SHS process, the raw materials Fe, NaClO{sub 4} (oxidizer), and NaCl (diluent) were thoroughly mixed in the desired ratio by ball milling, and the lower surfaces of the disk-shaped green compacts were subsequently electrically ignited to produce Fe{sub x}O through the propagation of the sustainable exothermic reaction. X-ray diffraction analysis showed that the SHS products comprised double phases of Fe{sub x}O and Fe{sub 3}O{sub 4}. The peaks of products with 0.947 {<=} x {<=} 1.00 shifted to lower angles in comparison to those of the product with x = 0.833 attributed to the lattice parameter distortion of the crystal structure because of the Fe defects. In the presence of the NaCl diluent, the raw materials were converted to high-purity Fe{sub x}O powders during the SHS process. Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating.

  6. Asymmetric synthesis of α-amino acids by reduction of N-tert-butanesulfinyl ketimine esters.

    Science.gov (United States)

    Reddy, Leleti Rajender; Gupta, Aditya P; Liu, Yugang

    2011-05-06

    A highly regio- and diastereoselective reduction of various N-tert-butanesulfinyl ketimine esters with L-Selectride resulting in the formation of α-amino acids is reported. This method is quite general and also practical for the preparation of both enantiomers of aryl or aliphatic α-amino acids in high yields. © 2011 American Chemical Society

  7. Multi-line split DNA synthesis: a novel combinatorial method to make high quality peptide libraries

    Directory of Open Access Journals (Sweden)

    Ueno Shingo

    2004-09-01

    Full Text Available Abstract Background We developed a method to make a various high quality random peptide libraries for evolutionary protein engineering based on a combinatorial DNA synthesis. Results A split synthesis in codon units was performed with mixtures of bases optimally designed by using a Genetic Algorithm program. It required only standard DNA synthetic reagents and standard DNA synthesizers in three lines. This multi-line split DNA synthesis (MLSDS is simply realized by adding a mix-and-split process to normal DNA synthesis protocol. Superiority of MLSDS method over other methods was shown. We demonstrated the synthesis of oligonucleotide libraries with 1016 diversity, and the construction of a library with random sequence coding 120 amino acids containing few stop codons. Conclusions Owing to the flexibility of the MLSDS method, it will be able to design various "rational" libraries by using bioinformatics databases.

  8. Molecular catalysis and high-volume organic synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Khidekel, M L; Vasserberg, V E

    1977-01-01

    The field of catalysis is very wide. The properties of catalysts are briefly reviewed and compared with the properties of enzymes. Various uses of enxymes in industry (sugar from corn, cellulose breakdown, etc.) are pointed out. The types of homogeneous and heterogeneous catalysts for use in organic synthesis are discussed. 48 refs. (SJR)

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

    African Journals Online (AJOL)

    NICO

    2011-02-25

    Feb 25, 2011 ... aFaculty of Chemistry, Bu-Ali Sina University, P.O. Box 651783868, Hamedan, Iran. ... Arylmethanes are useful compounds in organic synthesis and industry1 ... ketones,9,10 catalytic condensation of the Grignard reagent with.

  10. Digital synthesis of pulse shapes in real time for high resolution radiation spectroscopy

    International Nuclear Information System (INIS)

    Jordanov, Valentin T.; Knoll, Glenn F.

    1994-01-01

    Techniques have been developed for the synthesis of pulse shapes using fast digital schemes in place of the traditional analog methods of pulse shaping. Efficient recursive algorithms have been developed that allow real time implementation of a shaper that can produce either trapezoidal or triangular pulse shapes. Other recursive techniques are presented which allow a synthesis of finite cusp-like shapes. Preliminary experimental tests show potential advantages of using these techniques in high resolution, high count rate pulse spectroscopy. ((orig.))

  11. Synthesis and characterization of highly triboluminescent doped europium tetrakis compounds

    International Nuclear Information System (INIS)

    Fontenot, Ross S.; Hollerman, William A.; Bhat, Kamala N.; Aggarwal, Mohan D.

    2012-01-01

    One of the most intriguing properties involving crystals is their ability to emit light when fractured. While this property was discovered over 200 years ago, no one has ever been able to come up with a complete theory that can predict the physical principles associated with triboluminescence. However, this has not stopped scientists from coming up with various uses for these materials. One such application is to use these materials as the active element for smart impact sensors that can warn of catastrophic impacts. If these sensors are to become a reality however, the material must emit a bright light when fractured. One of the brightest triboluminescent materials found thus far is europium dibenzoylmethide triethylammonium (EuD 4 TEA). This material was discovered by Hurt in 1966 and is bright enough to be seen in daylight. In 2011, the authors discovered that synthesizing EuD 4 TEA using europium nitrate instead of chloride significantly increased the triboluminescence yield and made the synthesis much easier and more consistent. However, to date, there are few investigations into the effects of dopants on the triboluminescence of EuD 4 TEA. This paper reports the investigation of the effects of various dopants on: (1) The triboluminescent light yield, (2) Crystal size and structure, (3) Synthesis time, and (4) Prompt decay time. Results show that inclusion of dopants during synthesis increases the triboluminescence emission of EuD 4 TEA by 55%, significantly reduces the synthesis time, and controls the decay time. All of these properties can be useful for constructing the first prototype of a customized impact sensor. - Highlights: ► Doped europium dibenzoylmethide triethylammonium (EuD 4 TEA) was synthesized. ► Effects of dopants was studied from EuD 4 TEA during low velocity (<10 m/s) impacts. ► The triboluminescent light yield, decay time, and synthesis time were measured. ► A specially-built drop tower was developed to measure triboluminescence

  12. A self-propagation high-temperature synthesis and annealing route to synthesis of wave-like boron nitride nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jilin; Zhang, Laiping [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Gu, Yunle, E-mail: ncm@mail.wit.edu.cn [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Pan, Xinye; Zhao, Guowei; Zhang, Zhanhui [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China)

    2013-03-15

    Highlights: ► Large quantities of wave-like BN nanotubes were synthesized by SHS-annealing method. ► The catalytic boron-containing porous precursor was produced by self-propagation high-temperature synthesis method. ► Three growth models were proposed to explain the growth mechanism of the wave-like BN nanotubes. - Abstract: Large quantities of boron nitride (BN) nanotubes were synthesized by annealing a catalytic boron-containing porous precursor in flowing NH{sub 3} gas at 1180 °C. The porous precursor was prepared by self-propagation high-temperature synthesis (SHS) method at 800 °C using Mg, B{sub 2}O{sub 3} and amorphous boron powder (α-B) as the starting materials. The porous precursor played an important role in large quantities synthesis of BN nanotubes. The as-synthesized product was characterized by X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), Raman, Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM). Characterization results indicated that the BN nanotubes displayed wave-like inner structures with diameters in the range of 50–300 nm and average lengths of more than 10 μm. The possible growth mechanism of the BN nanotubes was also discussed.

  13. One-Pot Synthesis of 2-Acylindole-3-acetylketones via Domino Aza-alkylation/Michael Reaction Using o-Aminophenyl α,β-Unsaturated Ketones Followed by Desulfonative Dehydrogenation

    Energy Technology Data Exchange (ETDEWEB)

    Kim, A Reum; Yu, Mi Rim; Sim, Jong Tack; Kim, Sung Gon [Kyonggi Univ., Suwon (Korea, Republic of)

    2016-09-15

    The development of novel and practical synthetic methods with a minimum number of operations for the construction of bioactive structurally complex compounds is a major challenge in synthetic organic chemistry. Recently, we reported an efficient method for the stereoselective synthesis of 2,3-disubstituted indoline derivatives; cis-2,3-disubstituted indolines were obtained by the aza-alkylation/Michael cascade reaction of 2-(tosylamino)phenyl α,β-unsaturated ketones with α-bromoacetophenones in good yields and with excellent diastereoselectivities (Scheme 2, Eq. (1)). Among the available synthetic strategies, domino or cascade reactions have received wide acceptance as highly efficient and powerful methods for the synthesis of molecules with a high structural complexity. An efficient synthesis of 2,3-disubstituted indoles was developed by the domino aza-alkylation/intramolecular Michael reaction of 2-(tosylamino)phenyl α,β-unsaturated ketones with α-bromoacetophenones, followed by desulfonative dehydrogenation with DBU. The reaction afforded structurally diverse and highly functionalized 2,3-disubstituted indoles in moderate to excellent yields (up to 99%). The synthesis of 2,3-disubstituted indoles without desulfonation through DDQ-induced oxidative dehydrogenation was also achieved.

  14. Low Power Design with High-Level Power Estimation and Power-Aware Synthesis

    CERN Document Server

    Ahuja, Sumit; Shukla, Sandeep Kumar

    2012-01-01

    Low-power ASIC/FPGA based designs are important due to the need for extended battery life, reduced form factor, and lower packaging and cooling costs for electronic devices. These products require fast turnaround time because of the increasing demand for handheld electronic devices such as cell-phones, PDAs and high performance machines for data centers. To achieve short time to market, design flows must facilitate a much shortened time-to-product requirement. High-level modeling, architectural exploration and direct synthesis of design from high level description enable this design process. This book presents novel research techniques, algorithms,methodologies and experimental results for high level power estimation and power aware high-level synthesis. Readers will learn to apply such techniques to enable design flows resulting in shorter time to market and successful low power ASIC/FPGA design. Integrates power estimation and reduction for high level synthesis, with low-power, high-level design; Shows spec...

  15. NAA-modified DNA oligonucleotides with zwitterionic backbones: stereoselective synthesis of A-T phosphoramidite building blocks.

    Science.gov (United States)

    Schmidtgall, Boris; Höbartner, Claudia; Ducho, Christian

    2015-01-01

    Modifications of the nucleic acid backbone are essential for the development of oligonucleotide-derived bioactive agents. The NAA-modification represents a novel artificial internucleotide linkage which enables the site-specific introduction of positive charges into the otherwise polyanionic backbone of DNA oligonucleotides. Following initial studies with the introduction of the NAA-linkage at T-T sites, it is now envisioned to prepare NAA-modified oligonucleotides bearing the modification at X-T motifs (X = A, C, G). We have therefore developed the efficient and stereoselective synthesis of NAA-linked 'dimeric' A-T phosphoramidite building blocks for automated DNA synthesis. Both the (S)- and the (R)-configured NAA-motifs were constructed with high diastereoselectivities to furnish two different phosphoramidite reagents, which were employed for the solid phase-supported automated synthesis of two NAA-modified DNA oligonucleotides. This represents a significant step to further establish the NAA-linkage as a useful addition to the existing 'toolbox' of backbone modifications for the design of bioactive oligonucleotide analogues.

  16. Synthesis of tungstovanadophosphoric heteropolyacids and their behavior under high pressure

    International Nuclear Information System (INIS)

    Krasnoshchekov, V.V.; Morozova, P.P.

    1985-01-01

    By single-stage synthesis under elevated-pressures and temperatures (T=4 7 3 K, P=25000 atm) with 20-35% yield tungstovanadotophosphoric heteropoly acids (HPA) of different composition are prepared. The results of determining the compressibility, density and molecular volume of prepared HPA are given. It is shown that vanadium atoms introduction into tungstovanadium HPA molecule results in the decrease of density of the latter and increase of molar volumes

  17. Protecting-Group-Free Synthesis of 2-Deoxy-Aza-Sugars

    Directory of Open Access Journals (Sweden)

    Mattie Simon Maria Timmer

    2009-12-01

    Full Text Available The protecting-group-free asymmetric synthesis of 1,2,4-trideoxy-1,4-imino-L-xylitol is readily achieved in five steps from 2-deoxy-D-ribose and with an overall yield of 48%. Key in this synthesis is the application of our recently developed Vasella-reductive amination and carbamate annulation methodologies to the synthesis of 2-deoxy-aza-sugars. The carbamate annulation occurred with excellent yield and diastereoselectively (>20:1 d.r., in favour of the 3,4-cis isomer.

  18. Synthesis of highly faceted multiply twinned gold nanocrystals stabilized by polyoxometalates

    International Nuclear Information System (INIS)

    Yuan Junhua; Chen Yuanxian; Han Dongxue; Zhang Yuanjian; Shen Yanfei; Wang Zhijuan; Niu Li

    2006-01-01

    A novel and facile chemical synthesis of highly faceted multiply twinned gold nanocrystals is reported. The gold nanocrystals are hexagonal in transmission electron microscopy and icosahedral in scanning electron microscopy. Phosphotungstic acid (PTA), which was previously reduced, serves as a reductant and stabilizer for the synthesis of gold nanocrystals. The PTA-gold nanocomposites are quite stable in aqueous solutions, and electrochemically active towards the hydrogen evolution reaction

  19. Asimetric synthesis of alpha-phenyl amino acids; Sintesis asimetrica de alfa-fenilaminoacidos

    Energy Technology Data Exchange (ETDEWEB)

    Caltiviela, C.; Diaz de Villegas, M.D.; Galvez, J.A.; Lapena, Y. [Departamento de Quimica Organica, Universidad de Zaragoza, Zaragoza (Spain)

    1994-12-31

    A new synthetic strategy to obtain alpha-phenyl amino acids in enantiomerically pure form is described. The new route is based on the highly diastereoselective alkylation of (1S,2R,4R)-10-dicyclohexylsulfamoylisobornyl 2-phenylcianoacetate and subsequent curtis type rearrangement of the alkylated compound with total retention of configuration. 17 refs

  20. Product engineering by high-temperature flame synthesis

    DEFF Research Database (Denmark)

    Johannessen, Tue; Johansen, Johnny; Mosleh, Majid

    product gas can be applied directly in additional product engineering concepts. A brief overview of on-going product developments and product engineering projects is outlined below. These projects, which are all founded on flame synthesis of nano-structured materials, include: • Preparation of catalyzed...... hardware by direct deposition of catalysts on process equipment • Modifications of the substrate surfaces to obtain good adhesion during flame-coating • Formation of membrane layers by gas-phase deposition of nano-particles • Catalyst deposition in micro-reactors for rapid catalyst screening...

  1. Remote Stereoinductive Intramolecular Nitrile Oxide Cycloaddition: Asymmetric Total Synthesis and Structure Revision of (-)-11β-Hydroxycurvularin.

    Science.gov (United States)

    Choe, Hyeonjeong; Pham, Thuy Trang; Lee, Joo Yun; Latif, Muhammad; Park, Haeil; Kang, Young Kee; Lee, Jongkook

    2016-03-18

    The first total synthesis and structure revision of (-)-11β-hydroxycurvularin (1b), a macrolide possessing a β-hydroxyketone moiety, were accomplished. The β-hydroxyketone moiety in this natural product was introduced by cleavage of the N-O bond in an isoxazoline ring that was formed diastereoselectively in a 1,5-remote stereocontrolled fashion by employing intramolecular nitrile oxide cycloaddition.

  2. Highly Efficient Procedure for the Synthesis of Fructone Fragrance Using a Novel Carbon based Acid

    Directory of Open Access Journals (Sweden)

    Xuezheng Liang

    2010-08-01

    Full Text Available The novel carbon based acid has been synthesized via one-step hydrothermal carbonization of furaldehyde and hydroxyethylsulfonic acid. A highly efficient procedure for the synthesis of fructone has been developed using the novel carbon based acid. The results showed that the catalyst possessed high activity for the reaction, giving a yield of over 95%. The advantages of high activity, stability, reusability and low cost for a simple synthesis procedure and wide applicability to various diols and β-keto esters make this novel carbon based acid one of the best choices for the reaction.

  3. Prodigious Effects of Concentration Intensification on Nanoparticle Synthesis: A High-Quality, Scalable Approach

    KAUST Repository

    Williamson, Curtis B.

    2015-12-23

    © 2015 American Chemical Society. Realizing the promise of nanoparticle-based technologies demands more efficient, robust synthesis methods (i.e., process intensification) that consistently produce large quantities of high-quality nanoparticles (NPs). We explored NP synthesis via the heat-up method in a regime of previously unexplored high concentrations near the solubility limit of the precursors. We discovered that in this highly concentrated and viscous regime the NP synthesis parameters are less sensitive to experimental variability and thereby provide a robust, scalable, and size-focusing NP synthesis. Specifically, we synthesize high-quality metal sulfide NPs (<7% relative standard deviation for Cu2-xS and CdS), and demonstrate a 10-1000-fold increase in Cu2-xS NP production (>200 g) relative to the current field of large-scale (0.1-5 g yields) and laboratory-scale (<0.1 g) efforts. Compared to conventional synthesis methods (hot injection with dilute precursor concentration) characterized by rapid growth and low yield, our highly concentrated NP system supplies remarkably controlled growth rates and a 10-fold increase in NP volumetric production capacity (86 g/L). The controlled growth, high yield, and robust nature of highly concentrated solutions can facilitate large-scale nanomanufacturing of NPs by relaxing the synthesis requirements to achieve monodisperse products. Mechanistically, our investigation of the thermal and rheological properties and growth rates reveals that this high concentration regime has reduced mass diffusion (a 5-fold increase in solution viscosity), is stable to thermal perturbations (64% increase in heat capacity), and is resistant to Ostwald ripening.

  4. Synthesis of Carbocyclic Hydantocidins via Regioselective and Diastereoselective Phosphine-Catalyzed [3 + 2]-Cycloadditions to 5-Methylenehydantoins

    Energy Technology Data Exchange (ETDEWEB)

    Pham, Tien Q.; Pyne, Stephen G.; Skelton, Brian W.; White, Allan H. (UWA); (Wollongong)

    2010-07-20

    The phosphine-catalyzed [3 + 2]-cycloaddition of 5-methylenehydantoins 4 with the ylides 5, derived from addition of tributylphosphine to the 2-butynoic acid derivatives, 6a-d, gives spiro-heterocyclic products. The camphor sultam derivative 6b gives optically active products. Noteable was that the ylides derived from ethyl 2-butynoate and the 3-(2-butynoyl)-1,3-oxazolidin-2-one derivatives 6c and 6d gave spiro-heterocyclic products with reverse regioselectivities. The N,N-dibenzylprotected cycloadduct has been converted to carbocyclic hydantocidin and 6,7-diepi-carbocyclic hydantocidin.

  5. Fast and inexpensive synthesis of pentacene with high yield using 6,13-pentacenequinone as precursor

    Science.gov (United States)

    Mota, María L.; Rodriguez, Bibiana; Carrillo, Amanda; Ambrosio, Roberto C.; Luque, Priscy A.; Mireles, Marcela; Vivaldo, Israel; Quevedo, Manuel A.

    2018-02-01

    Pentacene is an important semiconductor in the field of organic electronics. In this work is presented an alternative synthesis procedure to obtain pentacene from 6,13-pentacenequinone as a precursor. Synthesis of pentacene was performed in two reactions, Diels-Adler cycloaddition of 6,13-pentacenequinone followed by 6,13-pentacenequinone reduction to pentacene, employing LiAlH4 as reducing agent. The products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), 1H-Nuclear Magnetic Resonance Spectroscopy (1H-NMR), X-Ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Ultraviolet-Visible Spectroscopy (UV-VIS). In this work, 6,13-pentacenequinone was synthetized with a high yield (55%) using an alternative method. The optimization process resulted in an overall reduction of reaction time while exhibiting high yield. The method presented here provides an affordable pentacene synthesis route with high purity, which can be further applied for research and development of organic electronic applications.

  6. STUDY OF GRINDING PROCESS OF TITANIUM CARBIDE PRODUCED WITH SELF-PROPAGATING HIGH TEMPERATURE SYNTHESIS (SPHTS)

    International Nuclear Information System (INIS)

    Kovziridze, Z.; Tabatadze, G.; Donadze, G.; Lezhava, A.; Gventsadze, D.

    2006-01-01

    It is stated that the specific character of SPHTS-preparations of TiC_x consists in crystal lattice strength reflecting the condition of synthesis in ''burning wave''. The use of roentgenographic and other methods of analysis allows to estimate the effect of the conditions of synthesis, causing carbon sublattice defect on grinding intensity of TiC_x phases. Study of the kinetics of vibro-grinding of TiC_x-phases in ethanol and benzene medium allows to establish high grinding intensity of the phases close to stoichiometry and the possibility of high depresion powderds (S_s_p H'' 4.5-6 m"2/g). (author)

  7. Highly bacterial resistant silver nanoparticles: synthesis and antibacterial activities

    International Nuclear Information System (INIS)

    Chudasama, Bhupendra; Vala, Anjana K.; Andhariya, Nidhi; Mehta, R. V.; Upadhyay, R. V.

    2010-01-01

    In this article, we describe a simple one-pot rapid synthesis route to produce uniform silver nanoparticles by thermal reduction of AgNO 3 using oleylamine as reducing and capping agent. To enhance the dispersal ability of as-synthesized hydrophobic silver nanoparticles in water, while maintaining their unique properties, a facile phase transfer mechanism has been developed using biocompatible block co-polymer pluronic F-127. Formation of silver nanoparticles is confirmed by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-vis spectroscopy. Hydrodynamic size and its distribution are obtained from dynamic light scattering (DLS). Hydrodynamic size and size distribution of as-synthesized and phase transferred silver nanoparticles are 8.2 ± 1.5 nm (σ = 18.3%) and 31.1 ± 4.5 nm (σ = 14.5%), respectively. Antimicrobial activities of hydrophilic silver nanoparticles is tested against two Gram positive (Bacillus megaterium and Staphylococcus aureus), and three Gram negative (Escherichiacoli, Proteusvulgaris and Shigellasonnei) bacteria. Minimum inhibitory concentration (MIC) values obtained in the present study for the tested microorganisms are found much better than those reported for commercially available antibacterial agents.

  8. Highly bacterial resistant silver nanoparticles: synthesis and antibacterial activities

    Energy Technology Data Exchange (ETDEWEB)

    Chudasama, Bhupendra, E-mail: bnchudasama@gmail.co [Thapar University, School of Physics and Materials Science (India); Vala, Anjana K.; Andhariya, Nidhi; Mehta, R. V. [Bhavnagar University, Department of Physics (India); Upadhyay, R. V. [Charotar University of Science and Technology, P.D. Patel Institute of Applied Sciences (India)

    2010-06-15

    In this article, we describe a simple one-pot rapid synthesis route to produce uniform silver nanoparticles by thermal reduction of AgNO{sub 3} using oleylamine as reducing and capping agent. To enhance the dispersal ability of as-synthesized hydrophobic silver nanoparticles in water, while maintaining their unique properties, a facile phase transfer mechanism has been developed using biocompatible block co-polymer pluronic F-127. Formation of silver nanoparticles is confirmed by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-vis spectroscopy. Hydrodynamic size and its distribution are obtained from dynamic light scattering (DLS). Hydrodynamic size and size distribution of as-synthesized and phase transferred silver nanoparticles are 8.2 {+-} 1.5 nm ({sigma} = 18.3%) and 31.1 {+-} 4.5 nm ({sigma} = 14.5%), respectively. Antimicrobial activities of hydrophilic silver nanoparticles is tested against two Gram positive (Bacillus megaterium and Staphylococcus aureus), and three Gram negative (Escherichiacoli, Proteusvulgaris and Shigellasonnei) bacteria. Minimum inhibitory concentration (MIC) values obtained in the present study for the tested microorganisms are found much better than those reported for commercially available antibacterial agents.

  9. The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

    Energy Technology Data Exchange (ETDEWEB)

    Nishimura, Akira; Kawahara, Nobuhiro [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan); Takagi, Hiroshi, E-mail: hiro@bs.naist.jp [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan)

    2013-01-04

    Highlights: Black-Right-Pointing-Pointer NO is produced from L-arginine in response to elevated temperature in yeast. Black-Right-Pointing-Pointer Tah18 was first identified as the yeast protein involved in NO synthesis. Black-Right-Pointing-Pointer Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe-S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

  10. The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

    International Nuclear Information System (INIS)

    Nishimura, Akira; Kawahara, Nobuhiro; Takagi, Hiroshi

    2013-01-01

    Highlights: ► NO is produced from L-arginine in response to elevated temperature in yeast. ► Tah18 was first identified as the yeast protein involved in NO synthesis. ► Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe–S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

  11. Short time synthesis of high quality carbon nanotubes with high rates by CVD of methane on continuously emerged iron nanoparticles

    International Nuclear Information System (INIS)

    Bahrami, Behnam; Khodadadi, Abasali; Mortazavi, Yadollah; Esmaieli, Mohamad

    2011-01-01

    We report the variation of yield and quality of carbon nanotubes (CNTs) grown by chemical vapor deposition (CVD) of methane on iron oxide-MgO at 900-1000 deg. C for 1-60 min. The catalyst was prepared by impregnation of MgO powder with iron nitrate, dried, and calcined at 300 deg. C. As calcined and unreduced catalyst in quartz reactor was brought to the synthesis temperature in helium flow in a few minutes, and then the flow was switched to methane. The iron oxide was reduced to iron nanoparticles in methane, while the CNTs were growing. TEM micrographs, in accordance with Raman RBM peaks, indicate the formation of mostly single wall carbon nanotubes of about 1.0 nm size. High quality CNTs with I G /I D Raman peak ratio of 14.5 are formed in the first minute of CNTs synthesis with the highest rate. Both the rate and quality of CNTs degrades with increasing CNTs synthesis time. Also CNTs quality sharply declines with temperature in the range of 900-1000 deg. C, while the CNTs yield passes through a maximum at 950 deg. C. About the same CNTs lengths are formed for the whole range of the synthesis times. A model of continuous emergence of iron nanoparticle seeds for CNTs synthesis may explain the data. The data can also provide information for continuous production of CNTs in a fluidized bed reactor.

  12. Short time synthesis of high quality carbon nanotubes with high rates by CVD of methane on continuously emerged iron nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Bahrami, Behnam, E-mail: bahrami@email.sc.edu [Catalysis and Nanostructured Materials Research Laboratory, School of Chemical Engineering, University of Tehran, Tehran (Iran, Islamic Republic of); Nanoelectronics Centre of Excellence, University of Tehran, Tehran (Iran, Islamic Republic of); Khodadadi, Abasali [Catalysis and Nanostructured Materials Research Laboratory, School of Chemical Engineering, University of Tehran, Tehran (Iran, Islamic Republic of); Mortazavi, Yadollah, E-mail: mortazav@ut.ac.ir [Nanoelectronics Centre of Excellence, University of Tehran, Tehran (Iran, Islamic Republic of); Esmaieli, Mohamad [Nanoelectronics Centre of Excellence, University of Tehran, Tehran (Iran, Islamic Republic of)

    2011-09-15

    We report the variation of yield and quality of carbon nanotubes (CNTs) grown by chemical vapor deposition (CVD) of methane on iron oxide-MgO at 900-1000 deg. C for 1-60 min. The catalyst was prepared by impregnation of MgO powder with iron nitrate, dried, and calcined at 300 deg. C. As calcined and unreduced catalyst in quartz reactor was brought to the synthesis temperature in helium flow in a few minutes, and then the flow was switched to methane. The iron oxide was reduced to iron nanoparticles in methane, while the CNTs were growing. TEM micrographs, in accordance with Raman RBM peaks, indicate the formation of mostly single wall carbon nanotubes of about 1.0 nm size. High quality CNTs with I{sub G}/I{sub D} Raman peak ratio of 14.5 are formed in the first minute of CNTs synthesis with the highest rate. Both the rate and quality of CNTs degrades with increasing CNTs synthesis time. Also CNTs quality sharply declines with temperature in the range of 900-1000 deg. C, while the CNTs yield passes through a maximum at 950 deg. C. About the same CNTs lengths are formed for the whole range of the synthesis times. A model of continuous emergence of iron nanoparticle seeds for CNTs synthesis may explain the data. The data can also provide information for continuous production of CNTs in a fluidized bed reactor.

  13. Direct synthesis of highly porous interconnected carbon nanosheets and their application as high-performance supercapacitors.

    Science.gov (United States)

    Sevilla, Marta; Fuertes, Antonio B

    2014-05-27

    An easy, one-step procedure is proposed for the synthesis of highly porous carbon nanosheets with an excellent performance as supercapacitor electrodes. The procedure is based on the carbonization of an organic salt, i.e., potassium citrate, at a temperature in the 750-900 °C range. In this way, carbon particles made up of interconnected carbon nanosheets with a thickness of <80 nm are obtained. The porosity of the carbon nanosheets consists essentially of micropores distributed in two pore systems of 0.7-0.85 nm and 0.95-1.6 nm. Importantly, the micropore sizes of both systems can be enlarged by simply increasing the carbonization temperature. Furthermore, the carbon nanosheets possess BET surface areas in the ∼1400-2200 m(2) g(-1) range and electronic conductivities in the range of 1.7-7.4 S cm(-1) (measured at 7.1 MPa). These materials behave as high-performance supercapacitor electrodes in organic electrolyte and exhibit an excellent power handling ability and a superb robustness over long-term cycling. Excellent results were obtained with the supercapacitor fabricated from the material synthesized at 850 °C in terms of both gravimetric and volumetric energy and power densities. This device was able to deliver ∼13 Wh kg(-1) (5.2 Wh L(-1)) at an extremely high power density of 78 kW kg(-1) (31 kW L(-1)) and ∼30 Wh kg(-1) (12 Wh L(-1)) at a power density of 13 kW kg(-1) (5.2 kW L(-1)) (voltage range of 2.7 V).

  14. Synthesis of hydroxide type sorbents from industry high-iron wastes

    International Nuclear Information System (INIS)

    Stepanenko, E.K.; Smirnov, A.L.

    1986-01-01

    Article presents the results of studies on possibility of using of technological iron containing wastes for the obtaining of hydroxide type sorbents in granular form. The scheme of technology of synthesis of hydroxide type sorbents from high-iron wastes is elaborated.

  15. Fast nanostructured carbon microparticle synthesis by one-step high-flux plasma processing

    NARCIS (Netherlands)

    Aussems, D. U. B.; Bystrov, K.; Dogan, I.; Arnas, C.; Cabié, M.; Neisius, T.; Rasinski, M.; Zoethout, E.; Lipman, P.; van de Sanden, M. C. M.; Morgan, T. W.

    2017-01-01

    This study demonstrates a fast one-step synthesis method for nanostructured carbon microparticles on graphite samples using high-flux plasma exposure. These structures are considered as potential candidates for energy applications such as Li-ion batteries and supercapacitors. The samples were

  16. Fast nanostructured carbon microparticle synthesis by one-step high-flux plasma processing

    NARCIS (Netherlands)

    Aussems, D.U.B.; Bystrov, K.E.; Doǧan, I.; Arnas, C.; Cabié, M.; Neisius, T.; Rasinski, M.; Lipman, P.J.L.; van de Sanden, M.C.M.; Morgan, T.W.

    This study demonstrates a fast one-step synthesis method for nanostructured carbon microparticles on graphite samples using high-flux plasma exposure. These structures are considered as potential candidates for energy applications such as Li-ion batteries and supercapacitors. The samples were

  17. Rational synthesis of zerovalent iron/bamboo charcoal composites with high saturation magnetization

    Science.gov (United States)

    Mingshan Wu; Jianfeng Ma; Zhiyong Cai; Genlin Tian; Shumin Yang; Youhong Wang; Xing' e Liu

    2015-01-01

    The synthesis of magnetic biochar composites is a major new research area in advanced materials sciences. A series of magnetic bamboo charcoal composites (MBC800, MBC1000 and MBC1200) with high saturation magnetization (Ms) was fabricated in this work by mixing bamboo charcoal powder with an aqueous ferric chloride solution and subsequently...

  18. Gel–sol synthesis and aging effect on highly crystalline anatase ...

    Indian Academy of Sciences (India)

    Gel–sol synthesis and aging effect on highly crystalline anatase nanopowder .... −1 in static air. To identify the gel-phase, it was mixed with D2O to form sample solution ... Ti(OH)4 chemical composition is produced this way: Ti3. [. (OC2H4)3 N. ].

  19. Synthesis of high specific active tritiated Leu-enkephalin in the leucine residue

    Energy Technology Data Exchange (ETDEWEB)

    Baba, S.; Hasegawa, H.; Shinohara, Y. (Tokyo Coll. of Pharmacy (Japan))

    1989-12-01

    Leu-enkephalin labelled with tritium in the Leu residue has been prepared. Synthesis of the precursor peptide, (4,5-dehydroLeu{sup 5}-)Leu-enkephalin, was carried out by solid phase synthesis using Fmoc amino acid derivatives. The peptide was tritiated catalytically yielding {sup 3}H-Leu-enkephalin with a specific radioactivity of 4.39 TBq/mmol. The distribution of tritium label was investigated by reversed-phase high performance liquid chromatography with a synchronized accumulating radioisotope detector following acidic and enzymatic hydrolysis, which confirmed that the tritium label was entirely located at the Leu residue. (author).

  20. Enantioselective synthesis of alpha,beta-disubstituted-beta-amino acids.

    Science.gov (United States)

    Sibi, Mukund P; Prabagaran, Narayanasamy; Ghorpade, Sandeep G; Jasperse, Craig P

    2003-10-01

    Highly diastereoselective and enantioselective addition of N-benzylhydroxylamine to imides 17 and 20-30 produces alpha,beta-trans-disubstituted N-benzylisoxazolidinones 19 and 31-41. These reactions proceed in 60-96% ee with 93-99% de's using 5 mol % of Mg(NTf2)2 and ligand 18. The product isoxazolidinones can be hydrogenolyzed directly to provide alpha,beta-disubstituted-beta-amino acids.

  1. New chiral phosphinephosphinite ligands: Application to stereoselective synthesis of a key intermediate of 1{beta}-methyl carbapenems by Rh(I)-catalyzed asymmetric hydroformylation

    Energy Technology Data Exchange (ETDEWEB)

    Saito, Takao; Yoshida, Akifumi; Matsumura, Kazuhiko [Takasago International Corp., Kanagawa (Japan)] [and others

    1995-12-31

    Transition metal catalyzed asymmetric hydroformylation is an attractive and highly useful homologation process for organic synthesis. Recently, the authors reported that the Rh(I) complexes of phosphinephosphite BINAPHOS are highly efficient catalysts for enantioselective hydroformylation of a variety of olefins. This time, the authors have designed and synthesized new chiral phosphinephosphinite ligands having binaphthyl backbone, (R)-2-diarylphosphino-2{prime}-diarylphosphinoxy-1,1{prime}-binaphthy1 (hereafter abbreviated (R)-BIPNITE). The Rh(I) complexes of these ligands are effective catalysts for the asymmetric hydroformylation of 4-vinylazetidin-2-one to give the corresponding oxo-aldehyde 3{beta} as the major product in very high diastereoselectivities and in good regioselectivities. Interestingly, modifications of the aryl substituents in phosphine and phosphinite moieties afforded higher selectivities. Aldehyde 3{beta} was easily oxidized with NaClO{sub 2} to 4, a key intermediate of 1{beta}-methyl carbapenems. Thus, the present method provides a new practical route to a versatile key intermediate for the synthesis of carbapenem antibiotics.

  2. Studies toward the asymmetric synthesis of the right part of the mycalamides.

    Science.gov (United States)

    Zhong, H Marlon; Sohn, Jeong-Hun; Rawal, Viresh H

    2007-01-19

    Described herein is the asymmetric synthesis of a functionalized, trioxadecalin unit that comprises the right-hand part of the mycalamides and related natural products. The synthetic route involves a 16-step sequence that accomplishes the formation of two heterocyclic rings and the generation of five stereocenters. The synthesis commenced with a C2-symmetric starting material, diethyl D-tartrate, and took advantage of a relay of diastereoselective reactions to extend this four-carbon chain and introduce new chiral centers. Subsequent electrophile-mediated cyclization afforded the desired pyran ring, which was then transformed into the desired, functionalized trioxadecalin skeleton.

  3. Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

    International Nuclear Information System (INIS)

    Kumar, Nikhil; Upadhyay, Lata Sheo Bachan

    2016-01-01

    Highlights: • A facile and eco-friendly method for the synthesis of L-cysteine functionalized copper nanoparticles is reported. • Synthesis of Highly stable L-cysteine functionalized copper nanoparticles (∼40 nm) was done in an aqueous medium. • FTIR analysis shows that L-cysteine bound to the nanoparticle surface via thiol group. - Abstract: A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month

  4. Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Nikhil, E-mail: nkumar.phd2011.bt@nitrr.ac.in; Upadhyay, Lata Sheo Bachan, E-mail: contactlataupadhyay@gmail.com

    2016-11-01

    Highlights: • A facile and eco-friendly method for the synthesis of L-cysteine functionalized copper nanoparticles is reported. • Synthesis of Highly stable L-cysteine functionalized copper nanoparticles (∼40 nm) was done in an aqueous medium. • FTIR analysis shows that L-cysteine bound to the nanoparticle surface via thiol group. - Abstract: A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month.

  5. Synthesis of nano-particle and highly porous conducting perovskites ...

    Indian Academy of Sciences (India)

    Administrator

    State Key Laboratory of Materials-oriented Chemical Engineering, Nanjing University of Technology,. No. 5 Xin Mofan Road, ... the molecule level mixing of the raw materials. The solid ... which were then calcined at 1000°C to form highly.

  6. High pressure synthesis of amorphous TiO2 nanotubes

    Directory of Open Access Journals (Sweden)

    Quanjun Li

    2015-09-01

    Full Text Available Amorphous TiO2 nanotubes with diameters of 8-10 nm and length of several nanometers were synthesized by high pressure treatment of anatase TiO2 nanotubes. The structural phase transitions of anatase TiO2 nanotubes were investigated by using in-situ high-pressure synchrotron X-ray diffraction (XRD method. The starting anatase structure is stable up to ∼20GPa, and transforms into a high-density amorphous (HDA form at higher pressure. Pressure-modified high- to low-density transition was observed in the amorphous form upon decompression. The pressure-induced amorphization and polyamorphism are in good agreement with the previous results in ultrafine TiO2 nanoparticles and nanoribbons. The relationship between the LDA form and α-PbO2 phase was revealed by high-resolution transmission electron microscopy (HRTEM study. In addition, the bulk modulus (B0 = 158 GPa of the anatase TiO2 nanotubes is smaller than those of the corresponding bulks and nanoparticles (180-240 GPa. We suggest that the unique open-ended nanotube morphology and nanosize play important roles in the high pressure phase transition of TiO2 nanotubes.

  7. Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

    Science.gov (United States)

    Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

    2016-02-01

    Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles.

  8. Pulsed high energy synthesis of fine metal powders

    Science.gov (United States)

    Witherspoon, F. Douglas (Inventor); Massey, Dennis W. (Inventor)

    1999-01-01

    Repetitively pulsed plasma jets generated by a capillary arc discharge at high stagnation pressure (>15,000 psi) and high temperature (>10,000 K) are utilized to produce 0.1-10 .mu.m sized metal powders and decrease cost of production. The plasma jets impact and atomize melt materials to form the fine powders. The melt can originate from a conventional melt stream or from a pulsed arc between two electrodes. Gas streams used in conventional gas atomization are replaced with much higher momentum flux plasma jets. Delivering strong incident shocks aids in primary disintegration of the molten material. A series of short duration, high pressure plasma pulses fragment the molten material. The pulses introduce sharp velocity gradients in the molten material which disintegrates into fine particles. The plasma pulses have peak pressures of approximately one kilobar. The high pressures improve the efficiency of disintegration. High gas flow velocities and pressures are achieved without reduction in gas density. Repetitively pulsed plasma jets will produce powders with lower mean size and narrower size distribution than conventional atomization techniques.

  9. Synthesis and stability of hydrogen selenide compounds at high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Pace, Edward J.; Binns, Jack; Alvarez, Miriam Pena; Dalladay-Simpson, Philip; Gregoryanz, Eugene; Howie, Ross T. (Edinburgh); (CHPSTAR- China)

    2017-11-14

    The observation of high-temperature superconductivity in hydride sulfide (H2S) at high pressures has generated considerable interest in compressed hydrogen-rich compounds. High-pressure hydrogen selenide (H2Se) has also been predicted to be superconducting at high temperatures; however, its behaviour and stability upon compression remains unknown. In this study, we synthesize H2Se in situ from elemental Se and molecular H2 at pressures of 0.4 GPa and temperatures of 473 K. On compression at 300 K, we observe the high-pressure solid phase sequence (I-I'-IV) of H2Se through Raman spectroscopy and x-ray diffraction measurements, before dissociation into its constituent elements. Through the compression of H2Se in H2 media, we also observe the formation of a host-guest structure, (H2Se)2H2, which is stable at the same conditions as H2Se, with respect to decomposition. These measurements show that the behaviour of H2Se is remarkably similar to that of H2S and provides further understanding of the hydrogen chalcogenides under pressure.

  10. Synthesis and characterization of highly purified nanosilica from pyrophyllite ores

    Energy Technology Data Exchange (ETDEWEB)

    Fuad, Abdulloh, E-mail: abdulloh.fuad.fmipa@um.ac.id; Mufti, Nandang; Diantoro, Markus; Subakti,; Septa Kurniawati, S. [Jurusan Fisika FMIPA Universitas Negeri Malang. Jl. Semarang No. 5 Malang, east Java (Indonesia)

    2016-03-11

    A simple method based on alkaline extraction followed by acid precipitation and acid dissolution has been developed to produce highly purified nanosilica from pyrophyllite materials. The reaction parameters such as molar ratio NaOH/SiO{sub 2}, reaction time and reaction temperature are varied for obtaining maximum nanosilica convertion. About 99,45% highly purified precipitated nanosilica measure with ICP, 259 m{sup 2}/gr measure with BET surface area, 97% whiteness and 3 ml/gr oil absorbtion from pyrophyllite materials has been achieved in closed system at 150°C within 180 min. The physicals and chemical properties (such as X-Ray Diffraction from PANalytical, X-Ray Fluorescence Minipal4 from PANanalytical, BET surface area, Forier Transform Infra Red Spectroscopy from Hitachi, and SEM-EDS Inspect-S50 from FEI Company) of the highly purity nanosilica were studied.

  11. Synthesis of high specific activity tritium labelled [2-3H]-adenosine-5'-triphosphate

    International Nuclear Information System (INIS)

    Jaiswal, D.K.; Morimoto, H.; Trump, E.L.; Williams, P.G.; Wemmer, D.E.

    1996-01-01

    A procedure for high level tritium labelling at the C2-H position of adenosine 5'-triphosphate ([2- 3 H]-ATP, 1), based on the tritiodehalogenation reaction of 2-bromoadenosine 5'-triphosphate (2) has been elaborated. This precursor was prepared in a six-step synthesis from guanosine. The tritiodehalogenation of (2) for three hours over palladium oxide in phosphate buffer yielded tritium labelled ATP with high specific activity, in good chemical yield. (author)

  12. Environmentally friendly synthesis of highly monodisperse biocompatible gold nanoparticles with urchin-like shape.

    Science.gov (United States)

    Lu, Lehui; Ai, Kelong; Ozaki, Yukihiro

    2008-02-05

    We report a facile and environmentally friendly strategy for high-yield synthesis of highly monodisperse gold nanoparticles with urchin-like shape. A simple protein, gelatin, was first used for the control over shape and orientation of the gold nanoparticles. These nanoparticles, ready to use for biological systems, are promising in the optical imaging-based disease diagnostics and therapy because of their tunable surface plasmon resonance (SPR) and excellent surface-enhanced Raman scattering (SERS) activity.

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

    Directory of Open Access Journals (Sweden)

    Gastón Silveira-Dorta

    2016-05-01

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

  14. Synthesis of a tritiated herbicide with high activity: methyl thifensulfuron

    International Nuclear Information System (INIS)

    Bastide, J.; Ortega, F.

    1993-01-01

    In order to study the binding on acetolactate synthase, a tritiated herbicide sulfonylurea (thifensulfuron methyl) of high specific activity was synthesized. By use of C 3 H 3 I for esterification of an acid group, a rapid incorporation of tritium into this compound may be achieved. (Author)

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

    Indian Academy of Sciences (India)

    bDepartment of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, P.O. Box 91775, ... key advantages of this process are high yields, shorter reaction times, easy work-up, ... ing pyran derivatives and hydrazine hydrate,9 use of.

  16. High quality voice synthesis middle ware; Kohinshitsu onsei gosei middle war

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2000-03-01

    Toshiba Corp. newly developed a natural voice synthesis system, TOS Drive TTS (TOtally speaker Driven Text-To-Speech) system, in which natural high-quality read-aloud is greatly improved, and also developed as its application a voice synthesis middle ware. In the newly developed system, using as a model a narrator's voice recorded preliminarily, a metrical control dictionary is automatically learned that reproduces the characteristics of metrical patters such as intonation or rhythm of a human voice, as is a voice bases dictionary that reproduces the characteristics of a voice quality, enabling natural voice synthesis to be realized that picks up human voice characteristics. The system is high quality and also very compact, while the voice synthesis middle ware utilizing this technology is adaptable to various platforms such as MPU or OS. The system is very suitable for audio response in the ITS field having car navigation systems as the core; besides, expanded application is expected to an audio response system that used to employ a sound recording and reproducing system. (translated by NEDO)

  17. High pressure synthesis of zeolite/polymer nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Haines, Julien; Thibaud, Jean-Marc; Rouquette, Jerome; Cambon, Olivier; Di Renzo, Francesco, E-mail: julien.haines@univ-montp2.fr [Institut Charles Gerhardt Montpellier (France); Lee, Arie van der [Institut Europeen des Membranes, Montpellier (France); Scelta, Demetrio; Ceppatelli, Matteo; Dziubek, Kamil; Gorelli, Federico; Bini, Roberto; Santoro, Mario [European Laboratory for Non Linear Spectroscopy, Firenze (Italy)

    2016-07-01

    Full text: Polymerization of simple organic molecules under high pressure in the subnanometric pores of pure SiO{sub 2} zeolites can be used to produce novel nanocomposite materials, which can be recovered at ambient P and have remarkable mechanical, electrical or optical properties. Polymerization of ethylene in silicalite was studied in situ at high pressure by IR and results in a nanocomposite with isolated chains of non-conducting polyethylene strongly confined in the pores based on single crystal x-ray diffraction data. The nanocomposite is much less compressible than silicalite and has a positive rather than a negative thermal expansion coefficient. In order to target novel electrical and optical properties, isolated chains of conducting polymers can also be prepared in the pores of zeolite hosts at high pressure, such as polyacetylene, which was polymerized under pressure in the pores of the 1-D zeolite TON. The structure of this nanocomposite was determined by synchrotron x-ray powder diffraction data with complete pore filling corresponding to one planar polymer chain confined in each pore with a zig-zag configuration in the yz plane. This very strong confinement can be expected to strongly modify the electrical properties of polyacetylene. In this nanocomposite, our theoretical calculations indicate that the electronic density of states of polyacetylene exhibit van Hove singularities related to quantum 1D confinement, which could lead to future technological applications. This new material is susceptible to have applications in nanoelectronics, nanophotonics and energy and light harvesting. Completely novel nanocomposites were prepared by the polymerization of carbon monoxide CO in silicalite and TON. In these materials, isolated, ideal polycarbonyl chains are obtained in contrast to the non-stoichiometric, branched bulk polymers obtained by high pressure polymerization of this simple system. These poly CO/zeolite composites could be interesting energetic

  18. Synthesis of aerogel tiles with high light scattering length

    CERN Document Server

    Danilyuk, A F; Okunev, A G; Onuchin, A P; Shaurman, S A

    1999-01-01

    The possibility of aerogel tiles production for RICH detectors is described. Monolithic blocks of silica aerogel were synthesized by two-step sol-gel processing of tetraethoxysilane Si(OEt) sub 4 followed by high temperature supercritical drying with organic solvent. The important characteristic of aerogel is the light scattering length. In the wide range of refraction indexes the light scattering length exceeds 4 cm at 400 nm.

  19. Large-Area Synthesis of High-Quality Uniform Few-Layer MoTe2.

    Science.gov (United States)

    Zhou, Lin; Xu, Kai; Zubair, Ahmad; Liao, Albert D; Fang, Wenjing; Ouyang, Fangping; Lee, Yi-Hsien; Ueno, Keiji; Saito, Riichiro; Palacios, Tomás; Kong, Jing; Dresselhaus, Mildred S

    2015-09-23

    The controlled synthesis of large-area, atomically thin molybdenum ditelluride (MoTe2) crystals is crucial for its various applications based on the attractive properties of this emerging material. In this work, we developed a chemical vapor deposition synthesis to produce large-area, uniform, and highly crystalline few-layer 2H and 1T' MoTe2 films. It was found that these two different phases of MoTe2 can be grown depending on the choice of Mo precursor. Because of the highly crystalline structure, the as-grown few-layer 2H MoTe2 films display electronic properties that are comparable to those of mechanically exfoliated MoTe2 flakes. Our growth method paves the way for the large-scale application of MoTe2 in high-performance nanoelectronics and optoelectronics.

  20. The course of protein synthesis during grain filling in normal and high lysine barley

    International Nuclear Information System (INIS)

    Giese, H.; Andersen, B.

    1984-01-01

    A study of the course of protein synthesis during grain filling in Bomi and the high lysine barleys Hily 82/3 and Risoe 56 showed that the four salt-soluble proteins, protein Z, β-amylase and the chymotrypsin inhibitors CI-1 and CI-2, are synthesized in greater amounts earlier in the high lysine lines than in Bomi. On the other hand, the hordeins are synthesized in greater amounts earlier during grain filling in Bomi than in Hily 82/3 and Risoe 56. There is no indication of a significant reduction of total protein synthesis in the high lysine lines compared with the standard lines Bomi and Pirrka. Hily 82/3 and Risoe 56 are very similar in protein composition in that they have a lower hordein content and higher levels, particularly of β-amylase and the chymotrypsin inhibitors, than Bomi. (author)

  1. Fabrication of Titanium Diboride-Cu Composite by Self-High Temperature Synthesis plus Quick Press

    Institute of Scientific and Technical Information of China (English)

    Jinyong ZHANG; Zhengyi FU; Weimin WANG

    2005-01-01

    Titanium diboride based composites, good candidates for contact materials, have high hardness, Young's modulus,high temperature stability, and excellent electrical, thermal conductivity. However a good interface of TiB2/Cu is very difficult to achieve for oxidation of TiB2. To avoid this oxidation behavior, the in situ combusting synthesis technology, SHS, was used to prepare TiB2/Cu composite. Thecharacters of Ti-B-xCu SHS were studied in detail,such as combustion temperature, products phases and grain size. Based on the experimental results a proper technology way of self-high temperature synthesis plus quick press (SHS/QP) was determined and compact TiB2/Cu composites with relative density over than 97 pct of the theoretical were fabricated by this method. The properties and microstructures of these TiB2 based composites were also investigated.

  2. Recent Advances in the Synthesis of High Explosive Materials

    Science.gov (United States)

    2015-12-29

    high thermal stability [29]. Unlike the blue copper(II) nitrotetrazole octahedral complex reported by Huynh [30], DBX-1 is the copper(I) salt that...II) nitrotetrazole octahedral complex reported by Huynh [30], DBX-1 is the copper(I) salt that manifests as orange-red crystals and adopts the...detonation velocity; i ΔfH0 = molar enthalpy of formation; j ΔexU0 = total energy of detonation. 3.3.3. Nitryl Cyanide (NCNO2) Though a simple

  3. High-yield synthesis and optical response of gold nanostars

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Pandian Senthil [Departamento de Quimica Fisica and Unidad Asociada CSIC-Universidade de Vigo, 36310 Vigo (Spain); Pastoriza-Santos, Isabel [Departamento de Quimica Fisica and Unidad Asociada CSIC-Universidade de Vigo, 36310 Vigo (Spain); RodrIguez-Gonzalez, Benito [Departamento de Quimica Fisica and Unidad Asociada CSIC-Universidade de Vigo, 36310 Vigo (Spain); Abajo, F Javier GarcIa de [Instituto de Optica-CSIC, Serrano 121, 28006 Madrid (Spain); Liz-Marzan, Luis M [Departamento de Quimica Fisica and Unidad Asociada CSIC-Universidade de Vigo, 36310 Vigo (Spain)

    2008-01-09

    Multipod Au nanoparticles (nanostars) with single crystalline tips were synthesized in extremely high yield through the reduction of HAuCl{sub 4} in a concentrated solution of poly(vinylpyrrolidone) (PVP) in N,N-dimethylformamide (DMF), in the presence of preformed Au nanoparticle seeds, but with no need for external energy sources. Nanostar dispersions display a well-defined optical response, which was found (through theoretical modeling) to comprise a main mode confined within the tips and a secondary mode confined in the central body. Calculations of the surface enhanced Raman scattering (SERS) response additionally show that this morphology will be relevant for sensing applications.

  4. High-yield synthesis and optical response of gold nanostars

    Science.gov (United States)

    Senthil Kumar, Pandian; Pastoriza-Santos, Isabel; Rodríguez-González, Benito; García de Abajo, F. Javier; Liz-Marzán, Luis M.

    2008-01-01

    Multipod Au nanoparticles (nanostars) with single crystalline tips were synthesized in extremely high yield through the reduction of HAuCl4 in a concentrated solution of poly(vinylpyrrolidone) (PVP) in N,N-dimethylformamide (DMF), in the presence of preformed Au nanoparticle seeds, but with no need for external energy sources. Nanostar dispersions display a well-defined optical response, which was found (through theoretical modeling) to comprise a main mode confined within the tips and a secondary mode confined in the central body. Calculations of the surface enhanced Raman scattering (SERS) response additionally show that this morphology will be relevant for sensing applications.

  5. High-yield synthesis and optical response of gold nanostars

    International Nuclear Information System (INIS)

    Kumar, Pandian Senthil; Pastoriza-Santos, Isabel; RodrIguez-Gonzalez, Benito; Abajo, F Javier GarcIa de; Liz-Marzan, Luis M

    2008-01-01

    Multipod Au nanoparticles (nanostars) with single crystalline tips were synthesized in extremely high yield through the reduction of HAuCl 4 in a concentrated solution of poly(vinylpyrrolidone) (PVP) in N,N-dimethylformamide (DMF), in the presence of preformed Au nanoparticle seeds, but with no need for external energy sources. Nanostar dispersions display a well-defined optical response, which was found (through theoretical modeling) to comprise a main mode confined within the tips and a secondary mode confined in the central body. Calculations of the surface enhanced Raman scattering (SERS) response additionally show that this morphology will be relevant for sensing applications

  6. Green Synthesis of Boron Carbonitride with High Capacitance

    Directory of Open Access Journals (Sweden)

    Dongping Chen

    2018-03-01

    Full Text Available Boron carbonitrides (BCN have attracted great interest in superhard or energy storage materials. In this work, thin BCN sheets were synthesized at 250 °C by a facile and green solvothermal method. The structure and morphology were characterized by X-ray diffraction (XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. Based on the results of electrochemical experiments, the thin BCN sheet exhibited excellent capacitance performance (343.1 F/g at a current density of 0.5 A/g and cycling stability (90%, which showed high potential applications in supercapacitors.

  7. Reduced graphene oxide synthesis by high energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Mondal, O. [Department of Physics, M.U.C Women' s College, Burdwan 713104 (India); Mitra, S. [MLS Prof' s Unit, Indian Association for the Cultivation of Science, Kolkata 700032 (India); Pal, M. [CSIR-Central Glass and Ceramic Research Institute, Kolkata 700032 (India); Datta, A. [University School of Basic and Applied Science (USBAS), Guru Gobind Singh Indraprastha University, New Delhi 110075 (India); Dhara, S. [Surface and Nanoscience Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India); Chakravorty, D., E-mail: mlsdc@iacs.res.in [MLS Prof' s Unit, Indian Association for the Cultivation of Science, Kolkata 700032 (India)

    2015-07-01

    Graphene oxide is transformed to reduced graphene oxide by high energy ball milling in inert atmosphere. The process of ball milling introduces defects and removes oxygen functional groups, thereby creating the possibility of fine tuning the band gap of all intermediate stages of the structural evolution. A limit of the backbone sp{sup 2} network structure has been found which should be able to accommodate defects, before amorphization sets in. The amorphization of graphene oxide is achieved rather quickly in comparison to that of graphite. From thermogravimetric and differential scanning calorimetric analysis along with Fourier transform infrared (FTIR) and Raman spectroscopic studies, it is found that the number of oxygen-containing groups decreases at a faster rate than that of aromatic double bonds with increasing ball milling time with a maximum limit of 3 h. Several characterization techniques (FTIR, Raman, UV–Visible and X-ray photoelectron spectroscopy) have confirmed that the material synthesized is, indeed, reduced graphene oxide. - Highlights: • Graphene oxide is transformed to reduced graphene oxide by high energy ball milling in inert atmosphere. • Fine tuning the band gap by introducing defects and removing oxygen functional groups. • Introduction of excess defects leads to amorphization. • Photoluminescence has been observed in the UV-blue region.

  8. New Synthesis and Tritium Labeling of a Selective Ligand for Studying High-Affinity γ-Hydroxybutyrate (GHB) Binding Sites

    DEFF Research Database (Denmark)

    Vogensen, Stine B.; Marek, Ales; Bay, Tina

    2013-01-01

    3-Hydroxycyclopent-1-enecarboxylic acid (HOCPCA, 1) is a potent ligand for the high-affinity GHB binding sites in the CNS. An improved synthesis of 1 together with a very efficient synthesis of [3H]-1 is described. The radiosynthesis employs in situ generated lithium trimethoxyborotritide. Screen...

  9. Science curriculum effects in high school: A quantitative synthesis

    Science.gov (United States)

    Weinstein, Thomas; Boulanger, F. David; Walberg, Herbert J.

    To assess the impact of the innovative precollege science curricula of the past twenty years on learning, a search was conducted using the computer-assisted Bibliographic Retrieval System (BRS), the ERIC Annual Summaries of Research in Science Education, and Dissertation Abstracts International. A total of 151 effect sizes were obtained from 33 studies representing 19,149 junior and senior high school students in the United States, Great Britain, and Israel. Study-weighted analysis yielded an overall mean effect size of 0.31 significantly favorable to the innovative curricula [t(25) = 2.183, p < 0.05] on all outcomes. Student performance in innovative curricula averaged in the 62nd percentile relative to the control norm. Tabulation of signed comparisons indicated that sixty-four out of eighty-one unweighted outcomes were favorable to the innovative curricula. Separate analyses for test content bias, methodological rigor, type of learning, and student characteristics showed no significant differences across these categories.

  10. Carbothermal shock synthesis of high-entropy-alloy nanoparticles

    Science.gov (United States)

    Yao, Yonggang; Huang, Zhennan; Xie, Pengfei; Lacey, Steven D.; Jacob, Rohit Jiji; Xie, Hua; Chen, Fengjuan; Nie, Anmin; Pu, Tiancheng; Rehwoldt, Miles; Yu, Daiwei; Zachariah, Michael R.; Wang, Chao; Shahbazian-Yassar, Reza; Li, Ju; Hu, Liangbing

    2018-03-01

    The controllable incorporation of multiple immiscible elements into a single nanoparticle merits untold scientific and technological potential, yet remains a challenge using conventional synthetic techniques. We present a general route for alloying up to eight dissimilar elements into single-phase solid-solution nanoparticles, referred to as high-entropy-alloy nanoparticles (HEA-NPs), by thermally shocking precursor metal salt mixtures loaded onto carbon supports [temperature ~2000 kelvin (K), 55-millisecond duration, rate of ~105 K per second]. We synthesized a wide range of multicomponent nanoparticles with a desired chemistry (composition), size, and phase (solid solution, phase-separated) by controlling the carbothermal shock (CTS) parameters (substrate, temperature, shock duration, and heating/cooling rate). To prove utility, we synthesized quinary HEA-NPs as ammonia oxidation catalysts with ~100% conversion and >99% nitrogen oxide selectivity over prolonged operations.

  11. Synthesis and properties of selenium trihydride at high pressures

    Science.gov (United States)

    Zhang, Xiao; Xu, Wan; Wang, Yu; Jiang, Shuqing; Gorelli, Federico A.; Greenberg, Eran; Prakapenka, Vitali B.; Goncharov, Alexander F.

    2018-02-01

    The chemical reaction products of molecular hydrogen (H2) with selenium (Se) are studied by synchrotron x-ray diffraction (XRD) and Raman spectroscopy at high pressures. We find that a common H2Se is synthesized at 0.3 GPa using laser heating. Upon compression at 300 K, a crystal of the theoretically predicted Cccm H3Se has been grown at 4.6 GPa. At room temperature, H3Se shows a reversible phase decomposition after laser irradiation above 8.6 GPa, but remains stable up to 21 GPa. However, at 170 K Cccm H3Se persists up to 39.5 GPa based on XRD measurements, while low-temperature Raman spectra weaken and broaden above 23.1 GPa. At these conditions, the sample is visually nontransparent and shiny suggesting that metallization occurred.

  12. New high performance nanoadditives for photocatalytic concrete: synthesis and study

    Directory of Open Access Journals (Sweden)

    FALIKMAN Vyacheslav Ruvimovich

    2015-02-01

    Full Text Available Nanotechnologies open up broad prospects for the creation of nanocatalysts, which are being more and more used in solving many problems associated with the protection of environment. Their behavior is directly related to the unique physical and chemical properties that are provided by quantum size effects, as well as the large specific surface area. It is known that the presence of photo catalysts in the construction segment of nanomaterials is becoming more prominent. One of the most significant achievements of the last years are photo catalytic active cement composites, including cements and concretes produced with the use of nanoparticles of titanium dioxide TiO₂ sensibilized through a nanotechnology . Currently they are widely used in practice to produce selfcleaning structures and to make clean an air of megacities. Further research in the field of development of new high-performance photo catalysts based on TiO₂ nanoparticles seems to be very relevant, because such R&D could significantly improve the technical characteristics of photo catalytic cements and concrete. In this paper an improved method to produce photo catalysts has been proposed. New synthesized products are based on TiO₂ nanoparticles applied on different inert carriers, including nanosilica. It was showed that these products can be used as a high performance photo catalyst in cement and cement-gypsum composites suitable for the onversion processes of nitric oxide and volatile organic substances, and air purification. It was determined that performance of the cementitious composites containing synthesized samples is 1,5…3,0 times higher than that for the commercial sample of the nanotitanium dioxide. The use of mechanical mixture of nanotitanium dioxide and inert supports is less effective and subjected to the «dilution law», in general.

  13. ACBC to Balcite: Bioinspired Synthesis of a Highly Substituted High-Temperature Phase from an Amorphous Precursor

    Energy Technology Data Exchange (ETDEWEB)

    Whittaker, Michael L.; Joester, Derk (NWU)

    2017-04-28

    Energy-efficient synthesis of materials locked in compositional and structural states far from equilibrium remains a challenging goal, yet biomineralizing organisms routinely assemble such materials with sophisticated designs and advanced functional properties, often using amorphous precursors. However, incorporation of organics limits the useful temperature range of these materials. Herein, the bioinspired synthesis of a highly supersaturated calcite (Ca0.5Ba0.5CO3) called balcite is reported, at mild conditions and using an amorphous calcium–barium carbonate (ACBC) (Ca1- x Ba x CO3·1.2H2O) precursor. Balcite not only contains 50 times more barium than the solubility limit in calcite but also displays the rotational disorder on carbonate sites that is typical for high-temperature calcite. It is significantly harder (30%) and less stiff than calcite, and retains these properties after heating to elevated temperatures. Analysis of balcite local order suggests that it may require the formation of the ACBC precursor and could therefore be an example of nonclassical nucleation. These findings demonstrate that amorphous precursor pathways are powerfully enabling and provide unprecedented access to materials far from equilibrium, including high-temperature modifications by room-temperature synthesis.

  14. Synthesis of multi-wavelength temporal phase-shifting algorithms optimized for high signal-to-noise ratio and high detuning robustness using the frequency transfer function

    OpenAIRE

    Servin, Manuel; Padilla, Moises; Garnica, Guillermo

    2016-01-01

    Synthesis of single-wavelength temporal phase-shifting algorithms (PSA) for interferometry is well-known and firmly based on the frequency transfer function (FTF) paradigm. Here we extend the single-wavelength FTF-theory to dual and multi-wavelength PSA-synthesis when several simultaneous laser-colors are present. The FTF-based synthesis for dual-wavelength PSA (DW-PSA) is optimized for high signal-to-noise ratio and minimum number of temporal phase-shifted interferograms. The DW-PSA synthesi...

  15. Concise Total Synthesis of (-)-Affinisine Oxindole, (+)-Isoalstonisine, (+)-Alstofoline, (-)-Macrogentine, (+)-Na -Demethylalstonisine, (-)-Alstonoxine A, and (+)-Alstonisine.

    Science.gov (United States)

    Stephen, Michael Rajesh; Rahman, M Toufiqur; Tiruveedhula, V V N Phani Babu; Fonseca, German O; Deschamps, Jeffrey R; Cook, James M

    2017-11-07

    A highly enantio- and diastereoselective strategy to access any member of the sarpagine/macroline family of oxindole alkaloids via internal asymmetric induction was developed from readily available d-(+)-tryptophan. At the center of this approach was the diastereospecific generation of the spiro[pyrrolidine-3,3'-oxindole] moiety at an early stage via a tert-butyl hypochlorite-promoted oxidative rearrangement of a chiral tetrahydro-β-carboline derivative. This key branching point determined the spatial configuration at the C-7 spiro center to be entirely 7R or 7S. Other key stereospecific processes were the asymmetric Pictet-Spengler reaction and Dieckmann cyclization, which were scalable to the 600 and 150 gram levels, respectively. Execution of this approach resulted in first enantiospecific total synthesis of (+)-isoalstonisine and (-)-macrogentine from the chitosenine series (7R), as well as (+)-alstonisine, (+)-alstofoline, (-)-alstonoxine A and (+)-N a -demethylalstonisine from the alstonisine series (7S). © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Controllable synthesis and characterization of highly fluorescent silver nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Li Junlin [Nanjing Normal University, School of Chemistry and Materials Science (China); An Xueqing, E-mail: anxueqin@ecust.edu.cn [East China University of Science and Technology, School of Chemistry and Molecular Engineering (China); Zhu Yinyan [Nanjing Normal University, School of Chemistry and Materials Science (China)

    2012-12-15

    Highly fluorescent silver nanoparticles (AgFNPs) have been prepared by microemulsion method and the sizes of AgFNPs were controlled by altering the molar ratio ({omega}) of water-to-surfactant in the water-in-oil microemulsion. The results were shown that the AgFNPs sizes increased with incremental molar ratio ({omega}) of water-to-surfactant. The AgFNPs have been characterized by transmission electron microscopy, dynamic light scattering, fluorescence and absorption spectroscopy, and fluorescence lifetime study. Study of the spectral characteristics was shown that the absorbance of AgFNPs increased significantly with the {omega}, and linear relationship between absorbance and the size of AgFNPs was observed. The increase of AgFNPs size caused a red shift of maximum absorption wavelength in the UV-Vis spectra, and the relationship between maximum absorption wavelength and AgFNPs size appeared linear dependence. The maximum fluorescence emission wavelength did not shift with the change of particles size, but the emission intensity increases with the {omega}. The results were shown that the other factors to affect the fluorescence properties of AgFNPs were the surface properties and microstructure, except the AgFNPs size. These surface properties depend upon the stabilizing agent, reactant concentration, and solvents and so on.

  17. Strategies for microbial synthesis of high-value phytochemicals

    Science.gov (United States)

    Li, Sijin; Li, Yanran; Smolke, Christina D.

    2018-03-01

    Phytochemicals are of great pharmaceutical and agricultural importance, but often exhibit low abundance in nature. Recent demonstrations of industrial-scale production of phytochemicals in yeast have shown that microbial production of these high-value chemicals is a promising alternative to sourcing these molecules from native plant hosts. However, a number of challenges remain in the broader application of this approach, including the limited knowledge of plant secondary metabolism and the inefficient reconstitution of plant metabolic pathways in microbial hosts. In this Review, we discuss recent strategies to achieve microbial biosynthesis of complex phytochemicals, including strategies to: (1) reconstruct plant biosynthetic pathways that have not been fully elucidated by mining enzymes from native and non-native hosts or by enzyme engineering; (2) enhance plant enzyme activity, specifically cytochrome P450 activity, by improving efficiency, selectivity, expression or electron transfer; and (3) enhance overall reaction efficiency of multi-enzyme pathways by dynamic control, compartmentalization or optimization with the host's metabolism. We also highlight remaining challenges to — and future opportunities of — this approach.

  18. A new reactivity mode for the diazo group: diastereoselective 1,3-aminoalkylation reaction of β-amino-α-diazoesters to give triazolines.

    Science.gov (United States)

    Kuznetsov, Alexey; Gulevich, Anton V; Wink, Donald J; Gevorgyan, Vladimir

    2014-08-18

    A novel mode of reactivity for the diazo group, the 1,3-addition of a nucleophile and an electrophile to the diazo group, has been realized in the intramolecular aminoalkylation of β-amino-α-diazoesters to form tetrasubstituted 1,2,3-triazolines. The reaction exhibited a broad scope, good functional group tolerance, and excellent diastereoselectivity. In addition, a new Au-catalyzed intramolecular transannulation reaction of the obtained propargyl triazolines to give pyrroles has been discovered. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Catalytic diastereoselective tandem conjugate addition-elimination reaction of Morita-Baylis-Hillman C adducts by C-C bond cleavage

    KAUST Repository

    Yang, Wenguo

    2012-02-08

    Through the cleavage of the C-C bond, the first catalytic tandem conjugate addition-elimination reaction of Morita-Baylis-Hillman C adducts has been presented. Various S N2′-like C-, S-, and P-allylic compounds could be obtained with exclusive E configuration in good to excellent yields. The Michael product could also be easily prepared by tuning the β-C-substituent group of the α-methylene ester under the same reaction conditions. Calculated relative energies of various transition states by DFT methods strongly support the observed chemoselectivity and diastereoselectivity. © 2012 Wiley-VCH Verlag GmbH&Co. KGaA, Weinheim.

  20. Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

    Science.gov (United States)

    Kumar, Nikhil; Upadhyay, Lata Sheo Bachan

    2016-11-01

    A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month

  1. Rapid continuous flow synthesis of high-quality silver nanocubes and nanospheres

    KAUST Repository

    Mehenni, Hakim

    2013-01-01

    We report a biphasic-liquid segmented continuous flow method for the synthesis of high-quality plasmonic single crystal silver nanocubes and nanospheres. The nanocubes were synthesized with controllable edge lengths from 20 to 48 nm. Single crystal nanospheres with a mean size of 29 nm were obtained by in-line continuous-flow etching of as-produced 39 nm nanocubes with an aqueous solution of FeNO3. In comparison to batch synthesis, the demonstrated processes represent highly scalable reactions, in terms of both production rate and endurance. The reactions were conducted in a commercially available flow-reactor system that is easily adaptable to industrial-scale production, facilitating widespread utilization of the procedure and the resulting nanoparticles. This journal is © The Royal Society of Chemistry 2013.

  2. Synthesis

    International Nuclear Information System (INIS)

    Voinis, Sylvie; Lalieux, Philippe; Thury, Marc; Horseman, Steve

    2001-01-01

    To prevent radioactive contamination and undue exposure to the public, it is required that long-lived and/or high-level radioactive wastes be isolated from the human environment for a very long period of time. For the purpose of isolating such wastes, the basic concept of deep disposal is to place packaged waste in a geological formation such as clay. One of main functions of the geological formation is to isolate waste from moving groundwater, thus minimising lixiviation of waste and advective radionuclide transport and, hence the amount of radionuclides that could reach the human environment. Improving our understanding of processes that might affect the containment properties of the geological barrier can reduce uncertainties about the performance of the repository. In particular, during the stepwise development of the research programme, it is important to clarify if fractures that might be induced by the excavation of the underground facilities might have a significant impact on the radiological safety of a repository in a host formation such as clay. In this framework, the self- healing properties of argillaceous media - often quoted as one of the advantages of such host formations - play a major role, notably in reducing the long-term impacts of such induced fracturing. Twenty-six participants representing several national waste management organisations, regulatory authorities, government agencies and the academic community from the OECD member countries and the EC took part in the Topical Session. The session was mainly aimed at exchanging information on: The general point of view on self-healing from geomechanical and geochemical experts; The approaches that are or will be followed by the various organisations in order to deal with the self-healing. The geological settings covered in the presentations related to the whole range of argillaceous media relevant to the disposal of radioactive wastes, including poorly indurated clays and indurated mud

  3. Design and synthesis of polymer, carbon and composite electrodes for high energy and high power supercapacitors

    Science.gov (United States)

    Arcila Velez, Margarita Rosa

    Supercapacitors (SCs) are promising energy storage devices because they deliver energy faster than Li-ion batteries and store larger amounts of charge compared to dielectric capacitors. SCs are classified in electrical double layer capacitors (EDLCs) and pseudocapacitors, based on their charge storage mechanism. EDLCs store charge electrostatically, i.e. by physical charge separation. This mechanism limits the storable amount of energy to the available surface area of the electrode, typically made of carbon materials, but grants good cycling stability of the SC device. Pseudocapacitor electrodes, commonly made of conducting polymers or metal oxides, store charge faradaically, i.e. through redox reactions throughout the bulk material, which allows them to store significantly larger amounts of energy than EDLCs, but their stability is compromised due to the partial irreversibility of the faradaic processes. To accomplish the commercialization of SCs, devices must show a combination of high charge storage capacities and long-term stability, besides being cost-effective. To tackle the current issues of SCs, this field of study has taken mainly two directions: 1) the development of new architectures and nanostructures of the active materials, which has shown to increase the surface area, enhance stability, and facilitate ion diffusion; and 2) fabrication of composites between non-faradaic (carbon), faradaic materials, and/or redox-active components to achieve a balance between the amount of energy stored and the stability. Following the first approach, a continuous process to grow vertically aligned carbon nanotubes (VACNTs) on cost-effective aluminum foil was developed. The resulting electrodes were analyzed as SC electrodes and in symmetric cells, and the influence of the arrangement of the nanotubes and the synthesis conditions was studied. The performance of the VACNTs produced continuously showed similar performance to the VACNTs produced stationarily and the

  4. Synthesis of [diene-"1"4C] curcumin at high specific activity

    International Nuclear Information System (INIS)

    Filer, Crist N.; Lacy, James M.; Wright, Christopher

    2016-01-01

    An efficient method is described to label curcumin with "1"4C at high specific activity. - Highlights: • This paper describes the synthesis of ["1"4C] Curcumin at the highest specific activity and total activity amount yet reported. • The "1"4C label was installed in the diene framework of Curcumin. • This paper also describes the characterization of ["1"4C] Curcumin by HPLC and mass spectrometry.

  5. Synthesis of high-surface-area spinel-type MgAl2O4 nanoparticles ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 1. Synthesis of high-surface-area spinel-type MgAl 2 O 4 nanoparticles by [Al(sal) 2 (H 2 O) 2 ] 2 [Mg(dipic) 2 ] and [Mg(H 2 O) 6 ][Al(ox) 2 (H 2 O) 2 ] 2 ·5H 2 O: influence of inorganic precursor type. Volume 40 Issue 1 February 2017 pp 45-53 ...

  6. Final Report on XStack: Software Synthesis for High Productivity ExaScale Computing

    Energy Technology Data Exchange (ETDEWEB)

    Solar-Lezama, Armando [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States). Computer Science and Artificial Intelligence Lab.

    2016-07-12

    The goal of the project was to develop a programming model that would significantly improve productivity in the high-performance computing domain by bringing together three components: a) Automated equivalence checking, b) Sketch-based program synthesis, and c) Autotuning. The report provides an executive summary of the research accomplished through this project. At the end of the report is appended a paper that describes in more detail the key technical accomplishments from this project, and which was published in SC 2014.

  7. Water-based synthesis of hydrophobic ionic liquids for high-energy electrochemical devices

    International Nuclear Information System (INIS)

    Montanino, Maria; Alessandrini, Fabrizio; Passerini, Stefano; Appetecchi, Giovanni Battista

    2013-01-01

    Highlights: ► Water-based synthesis of ionic liquids with high yield. ► Full recycling of reagents. ► High purity pyrrolidinium-based ionic liquids with exceptional electrochemical stability window. ► Lithium plating from pyrrolidinium-based ionic liquids. -- Abstract: In this work is described an innovative synthesis route for hydrophobic ionic liquids (ILs) composed of N-methyl-N-alkylpyrrolidinium (or piperidinium) or imidazolium or tetralkylammonium cations and (perfluoroalkylsulfonyl)imide, ((C n F 2n+1 SO 2 )(C m F 2m+1 SO 2 )N − ), anions. This synthesis does not require the use of any environmental unfriendly solvent such as acetone, acetonitrile or halogen-containing compounds, which is not welcome in industrial applications. Only water is used as the process solvent throughout the entire process. In addition, the commonly used iodine-containing reagents were replaced by the cheaper, more chemically stable and less toxic bromine-containing compounds. A particular care was devoted to the development of the purification route, which is especially important for ILs to be used in high-energy electrochemical devices such as high voltage supercapacitors and lithium batteries. The effect of the reaction temperature, the time and the stoichiometry in the various steps of the synthesis have been investigated in detail. This novel procedure allowed obtaining ultrapure (>99.9 wt.%), clear, colourless, inodorous ILs with an overall yield above 92 wt.% and moisture content below 1 ppm. NMR measurements were run to confirm the chemical structure whereas elemental analysis and electrochemical tests were performed to check the purity of the synthesized ILs

  8. Synthesis and characterization of strontium carboxylates at room temperature and at high temperature in autoclave vessels

    DEFF Research Database (Denmark)

    Christgau, Stephan; Ståhl, Kenny; Andersen, Jens Enevold Thaulov

    2006-01-01

    A novel method was developed for synthesis of strontium coordination compounds in high yields. The synthesis proceeded along three pathways that provided strontium salts in high purity and high yields, close to 100%, as confirmed by flame atomic absorption spectroscopy (FAAS) and powder x......-ray crystallography. Optimum conditions were found at T = 120-1400C, a base-to-acid ratio of 1.2 and 15 min. of reaction-time in an autoclave vessel. Large crystals were readily obtained within a time period of hours. The crystal structures of strontium D-glutamate hexahydrate (I) and strontium di-(hydrogen L......-glutamate) pentahydrate (II) were confirmed by X-ray powder diffraction at 295 K and Rietveld refinements (I: Space group P212121, Z=4, a=7.3519(2), b=8.7616(2), c=20.2627(5) Å, and II: Space group P21, Z=2, a=8.7243(1), b=7.2635(1), c=14.6840(2) Å, β=100.5414(7) °). Synthesis at room temperature provided four additional...

  9. T3P- A Novel Catalyst for Aza-Diels-Alder Reaction: One-Pot Synthesis of Pyrano[3,2-c]quinolines and furano[3,2-c]quinolines

    Directory of Open Access Journals (Sweden)

    T. S. R. Prasanna

    2011-01-01

    Full Text Available T3P was found to be an efficient catalyst for the Aza-Diels–Alder reactions of aldimines with dihydropyran or dihydrofuran to afford the corresponding pyrano-and furo [3,2-c]quinolines in high yields with high diastereoselectivity in a short period of time.

  10. High-concentration copper nanoparticles synthesis process for screen-printing conductive paste on flexible substrate

    International Nuclear Information System (INIS)

    Tam, Sze Kee; Ng, Ka Ming

    2015-01-01

    This study presents a method for the synthesis of copper nanoparticles, which are poised to replace silver nanoparticles in some application areas of printed electronics. This method offers three advantages. Firstly, copper loading in the synthesis reaction can be as high as 1 M, offering high productivity in large-scale production. Secondly, the size of the copper nanoparticles can be controlled from 12 to 99 nm. Thirdly, the surface polarity of the particles can be modified. Thus, a tailor-made product can be synthesized. The synthesis of copper nanoparticles coated with various capping agents, including dodecanethiol, lauric acid, nonanoic acid, polyacrylic acid, and polyvinyl pyrrolidone, was demonstrated. The nonanoic acid-coated copper nanoparticles were formulated as a screen-printing conductive paste. The particles were readily dispersed in terpineol, and the paste could be screen printed onto flexible polyester. The electrical resistivity of patterns after a low-temperature (120 °C) sintering treatment was around 5.8 × 10 −5  Ω cm.Graphical Abstract

  11. High-concentration copper nanoparticles synthesis process for screen-printing conductive paste on flexible substrate

    Energy Technology Data Exchange (ETDEWEB)

    Tam, Sze Kee; Ng, Ka Ming, E-mail: kekmng@ust.hk [The Hong Kong University of Science and Technology, Department of Chemical and Biomolecular Engineering (Hong Kong)

    2015-12-15

    This study presents a method for the synthesis of copper nanoparticles, which are poised to replace silver nanoparticles in some application areas of printed electronics. This method offers three advantages. Firstly, copper loading in the synthesis reaction can be as high as 1 M, offering high productivity in large-scale production. Secondly, the size of the copper nanoparticles can be controlled from 12 to 99 nm. Thirdly, the surface polarity of the particles can be modified. Thus, a tailor-made product can be synthesized. The synthesis of copper nanoparticles coated with various capping agents, including dodecanethiol, lauric acid, nonanoic acid, polyacrylic acid, and polyvinyl pyrrolidone, was demonstrated. The nonanoic acid-coated copper nanoparticles were formulated as a screen-printing conductive paste. The particles were readily dispersed in terpineol, and the paste could be screen printed onto flexible polyester. The electrical resistivity of patterns after a low-temperature (120 °C) sintering treatment was around 5.8 × 10{sup −5} Ω cm.Graphical Abstract.

  12. Highly uniform up-converting nanoparticles: Why you should control your synthesis even more

    International Nuclear Information System (INIS)

    Palo, Emilia; Tuomisto, Minnea; Hyppänen, Iko; Swart, Hendrik C.; Hölsä, Jorma; Soukka, Tero; Lastusaari, Mika

    2017-01-01

    Luminescent β-NaYF 4 :Yb 3+ ,Er 3+ (x Yb : 0.17, x Er : 0.03) nanomaterials were synthesized for use as labels for biomedical applications with high temperature co-precipitation synthesis in 1-octadecene and oleic acid. The effect of the synthesis conditions (e.g. argon flow, cooling and stirring rates) on the products’ up-conversion luminescence intensity, particle size and morphology were studied. The factors contributing to these properties were analysed. It was observed that an efficient inert gas flow is essential to the formation of the preferred highly-luminescent hexagonal structure. Furthermore, the flow rate, together with the stirring rate, crucially affect the Er:Yb molar ratio of the products. The optimization of this ratio is essential when strong up-conversion emission is required from small particles, whereas the morphology and uniformity of the nanoparticles can be controlled with the cooling rate. These results emphasize the importance of controlling the synthesis conditions, especially when nanoparticles need to have a specific morphology because of their use e.g. as luminescent labels in medical diagnostics.

  13. Highly uniform up-converting nanoparticles: Why you should control your synthesis even more

    Energy Technology Data Exchange (ETDEWEB)

    Palo, Emilia, E-mail: ekharj@utu.fi [University of Turku, Department of Chemistry, FI-20014 Turku (Finland); University of Turku Graduate School (UTUGS), Doctoral Programme in Physical and Chemical Sciences, Turku (Finland); Turku University Centre for Materials and Surfaces (MatSurf), Turku (Finland); Tuomisto, Minnea [University of Turku, Department of Chemistry, FI-20014 Turku (Finland); University of Turku Graduate School (UTUGS), Doctoral Programme in Physical and Chemical Sciences, Turku (Finland); Turku University Centre for Materials and Surfaces (MatSurf), Turku (Finland); Hyppänen, Iko [University of Turku, Department of Chemistry, FI-20014 Turku (Finland); Turku University Centre for Materials and Surfaces (MatSurf), Turku (Finland); Swart, Hendrik C.; Hölsä, Jorma [University of the Free State, Department of Physics, Bloemfontein ZA-9300 (South Africa); Soukka, Tero [University of Turku, Department of Biochemistry, FI-20014 Turku (Finland); Lastusaari, Mika [University of Turku, Department of Chemistry, FI-20014 Turku (Finland); Turku University Centre for Materials and Surfaces (MatSurf), Turku (Finland)

    2017-05-15

    Luminescent β-NaYF{sub 4}:Yb{sup 3+},Er{sup 3+} (x{sub Yb}: 0.17, x{sub Er}: 0.03) nanomaterials were synthesized for use as labels for biomedical applications with high temperature co-precipitation synthesis in 1-octadecene and oleic acid. The effect of the synthesis conditions (e.g. argon flow, cooling and stirring rates) on the products’ up-conversion luminescence intensity, particle size and morphology were studied. The factors contributing to these properties were analysed. It was observed that an efficient inert gas flow is essential to the formation of the preferred highly-luminescent hexagonal structure. Furthermore, the flow rate, together with the stirring rate, crucially affect the Er:Yb molar ratio of the products. The optimization of this ratio is essential when strong up-conversion emission is required from small particles, whereas the morphology and uniformity of the nanoparticles can be controlled with the cooling rate. These results emphasize the importance of controlling the synthesis conditions, especially when nanoparticles need to have a specific morphology because of their use e.g. as luminescent labels in medical diagnostics.

  14. Production of advanced materials by methods of self-propagating high-temperature synthesis

    CERN Document Server

    Tavadze, Giorgi F

    2013-01-01

    This translation from the original Russian book outlines the production of a variety of materials by methods of self-propagating high-temperature synthesis (SHS). The types of materials discussed include: hard, refractory, corrosion and wear-resistant materials, as well as other advanced and speciality materials. The authors address the issue of optimal parameters for SHS reactions occurring during processes involving a preliminary metallothermic reduction stage, and they calculate this using thermodynamic approaches. In order to confirm the effectiveness of this approach, the authors describe experiments focussing on the synthesis of elemental crysalline boron, boron carbides and nitrides. Other parts of this brief include theoretical and experimental results on single-stage production of hard alloys on the basis of titanium and zirconium borides, as well as macrokinetics of degassing and compaciton of SHS-products.This brief is suitable for academics, as well as those working in industrial manufacturing com...

  15. Synthesis of all-silica zeolites from highly concentrated gels containing hexamethonium cations

    KAUST Repository

    Liu, Xiaolong

    2012-07-01

    A pure and highly crystalline all-silica EU-1 zeolite has been obtained from the crystallization of gels containing very low water contents in the presence of hexamethonium cations. Decreasing the water content in the gel down to H 2O/Si < 1 inhibited the formation of ZSM-48, which is usually observed under more diluted standard crystallization conditions. Moreover, addition of NH 4F to the synthesis led to the formation of "half-fluorinated" ITQ-13 in which fluoride anions occupied only the center of D4R cages. In larger cages, the charge of the template was compensated by framework connectivity defects, clearly demonstrating once more the essential role of F - in the formation of D4R units. The formation of such hybrid (F,OH) is particularly interesting from a synthesis point of view, particularly for understanding the respective roles of fluoride and hydroxide anions in the crystallization process. © 2012 Elsevier Inc. All rights reserved.

  16. High-Throughput Platform for Synthesis of Melamine-Formaldehyde Microcapsules.

    Science.gov (United States)

    Çakir, Seda; Bauters, Erwin; Rivero, Guadalupe; Parasote, Tom; Paul, Johan; Du Prez, Filip E

    2017-07-10

    The synthesis of microcapsules via in situ polymerization is a labor-intensive and time-consuming process, where many composition and process factors affect the microcapsule formation and its morphology. Herein, we report a novel combinatorial technique for the preparation of melamine-formaldehyde microcapsules, using a custom-made and automated high-throughput platform (HTP). After performing validation experiments for ensuring the accuracy and reproducibility of the novel platform, a design of experiment study was performed. The influence of different encapsulation parameters was investigated, such as the effect of the surfactant, surfactant type, surfactant concentration and core/shell ratio. As a result, this HTP-platform is suitable to be used for the synthesis of different types of microcapsules in an automated and controlled way, allowing the screening of different reaction parameters in a shorter time compared to the manual synthetic techniques.

  17. Recent development on the synthesis of calixcrowns and their application for cesium removal from high-level liquid waste

    International Nuclear Information System (INIS)

    Zhu Xiaowen; Gao Jianxun; Wang Jianchen; Yu Bo; Song Chongli

    2002-01-01

    The synthesis, extraction properties and molecular modeling of calixcrowns in concern of cesium removal is reviewed briefly. In particular, calix [4] crown-6 and some of its derivatives have been shown to be highly selective extractants for cesium ions

  18. Studies on the Total Synthesis of Amphidinolide O (II): A Stereoselective Synthesis of C1-C11 Fragment

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Mi Yeon; Kim, Jong Woo; Lee, Duck Hyung [Sogang University, Seoul (Korea, Republic of)

    2005-10-15

    Two ketones and, the C1-C11 fragment of Amphidinolide O, were prepared stereoselectively via 14 and 16 step sequences in 8.7% and 2.0% overall yield, respectively. The amphidinolides were isolated from the marine dinoflagellate Amphidinium sp., which produces a host of secondary metabolites endowed with potent cytotoxicity against various cancer cell lines. Amphidinolide O displayed potent in vitro cytotoxicity against L1210 marine leukemia cells and human epidermoid carcinoma KB cells with 1.7 and 3.6 μg/mL of IC50s, respectively. In addition to our recent reports regarding to the synthesis of C12-C17 and C3-C11 fragments of amphidinolide O, we describe herein a new route to diastereoselective synthesis of C1-C11 fragment of. The retrosynthetic analysis of led to the C1-C11 fragment and C12-C17 fragment. The hemiketal was expected from acyclic precursor 4 which, in turn, would be derived by diastereoselective aldol reaction between ketone and aldehyde.

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

    Directory of Open Access Journals (Sweden)

    Ravi Bansal

    2017-05-01

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

  20. Highly Enantioselective Rhodium-Catalyzed Addition of Arylboroxines to Simple Aryl Ketones: Efficient Synthesis of Escitalopram.

    Science.gov (United States)

    Huang, Linwei; Zhu, Jinbin; Jiao, Guangjun; Wang, Zheng; Yu, Xingxin; Deng, Wei-Ping; Tang, Wenjun

    2016-03-24

    Highly enantioselective additions of arylboroxines to simple aryl ketones have been achieved for the first time with a Rh/(R,R,R,R)-WingPhos catalyst, thus providing a range of chiral diaryl alkyl carbinols with excellent ee values and yields. (R,R,R,R)-WingPhos has been proven to be crucial for the high reactivity and enantioselectivity. The method has enabled a new, concise, and enantioselective synthesis of the antidepressant drug escitalopram. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. High-Yield Synthesis of Zinc Oxide Nanoparticles from Bicontinuous Microemulsions

    Directory of Open Access Journals (Sweden)

    S. López-Cuenca

    2011-01-01

    Full Text Available The high-yield synthesis of zinc oxide (ZnO primary nanoparticles with high purity and with diameters between 6 and 22 nm using bicontinuous microemulsions is reported in this work. The ZnO nanoparticles were made by hydrolysis of Zn(NO32 with NaOH aqueous solution and precipitation, followed by calcination of the precipitate. Higher yields and productivities of ZnO nanoparticles were obtained compared to values produced with w/o micremulsions reported in the literature. Particles were characterized by transmission electronic microscopy (TEM, X-ray diffraction, and atomic absorption spectroscopy.

  2. High pressure synthesis of ThB/sub 12/ and HfB/sub 12/

    Energy Technology Data Exchange (ETDEWEB)

    Cannon, J F; Farnsworth, P B [Brigham Young Univ., Provo, UT (USA). Dept. of Chemistry

    1938-08-01

    High pressure synthesis techniques were used to prepare ThB/sub 12/ and HfB/sub 12/. These compounds have the cubic UB/sub 12/-type structure with lattice parameters 7.612(1) A and 7.377(2) A respectively. The relationship between the lattice parameter for UB/sub 12/-type dodecaborides and the coordination number 12 radius of the metal atom differs for lanthanide, actinide and transition metal atoms. The prediction is made that it is possible to prepare AmB/sub 12/ at high pressures.

  3. Stereoselective Synthesis of Tetrahydroindolizines through the Catalytic Formation of Pyridinium Ylides from Diazo Compounds.

    Science.gov (United States)

    Day, Jonathan; McKeever-Abbas, Ben; Dowden, James

    2016-05-04

    Commercially available iron(III) and copper(I) complexes catalyzed multicomponent cycloaddition reactions between diazo compounds, pyridines, and electrophilic alkenes to give alkaloid-inspired tetrahydroindolizidines in high yield with high diastereoselectivity. Hitherto, the catalytic formation of versatile pyridinium ylides from metal carbenes has been poorly developed; the broad utility demonstrated herein sets the stage for the invention of further multicomponent reactions in future. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. An enantiomerically pure siderophore type ligand for the diastereoselective 1 : 1 complexation of lanthanide(III ions

    Directory of Open Access Journals (Sweden)

    Markus Albrecht

    2009-12-01

    Full Text Available A facile synthesis of a highly preorganized tripodal enterobactine-type ligand 1a-H3 consisting of a chiral C3-symmetric macrocyclic peptide and three tridentate 2-amido-8-hydroxyquinoline coordinating units is presented. Complex formation with various metal ions (Al3+, Ga3+, Fe3+, La3+ and Eu3+ was investigated by spectrophotometric methods. Only in the case of La3+ and Eu3+ were well defined 1 : 1 complexes formed. On the basis of CD spectroscopy and DFT calculations the configuration at the metal centre of the La3+ complex was determined to show Λ helicity. The coordination compounds [(1aLn] presented should be prototypes for further lanthanide(III complexes with an enterobactine analogue binding situation.

  5. Multi-granularity synthesis segmentation for high spatial resolution Remote sensing images

    International Nuclear Information System (INIS)

    Yi, Lina; Liu, Pengfei; Qiao, Xiaojun; Zhang, Xiaoning; Gao, Yuan; Feng, Boyan

    2014-01-01

    Traditional segmentation method can only partition an image in a single granularity space, with segmentation accuracy limited to the single granularity space. This paper proposes a multi-granularity synthesis segmentation method for high spatial resolution remote sensing images based on a quotient space model. Firstly, we divide the whole image area into multiple granules (regions), each region is consisted of ground objects that have similar optimal segmentation scale, and then select and synthesize the sub-optimal segmentations of each region to get the final segmentation result. To validate this method, the land cover category map is used to guide the scale synthesis of multi-scale image segmentations for Quickbird image land use classification. Firstly, the image is coarsely divided into multiple regions, each region belongs to a certain land cover category. Then multi-scale segmentation results are generated by the Mumford-Shah function based region merging method. For each land cover category, the optimal segmentation scale is selected by the supervised segmentation accuracy assessment method. Finally, the optimal scales of segmentation results are synthesized under the guide of land cover category. Experiments show that the multi-granularity synthesis segmentation can produce more accurate segmentation than that of a single granularity space and benefit the classification

  6. Engineering high power induction plasma unit at BARC for mass synthesis of refractory nano-ceramics

    International Nuclear Information System (INIS)

    Ghorui, S.; Sahasrabudhe, S.N.; Dhamale, G.; Das, A.K.

    2013-01-01

    Atmospheric pressure RF thermal plasma sources are gaining increasing importance for production of high purity novel nano-materials in different high-end technological applications. Inherent electrode-less features of the discharge together with the large volume and high energy density of the produced plasma ensures contamination free process environment and mass production ability. Reported herewith is the development of an indigenous induction plasma system for mass synthesis of nanopowders of refractory ceramic materials. The system has been tested for continuous synthesis of Al 2 O 3 nano-powder at a rate of more than 600 gm per hour and checked for its viability for bulk production of nano-particles of other refractory ceramics like Yttrium oxide and Neodymium Oxide. From collected evidences, the process of formation of the nano-particles is identified as the evaporation and subsequent homogeneous nucleation. Major features observed for alumina are complete conversion into highly spherical nano-sized particles, small particle sizes, very narrow size distribution, highly crystallite nature and mixed phases depending on the zone of collection. For alumina, the particles are found to exhibit a uni-modal distribution with peak near 15 nm

  7. Fe-Catalyzed Synthesis of Porous Carbons Spheres with High Graphitization Degree for High-Performance Supercapacitors

    Science.gov (United States)

    Zhu, Jun; Shi, Hongwei; Zhuo, Xin; Hu, Yalin

    2017-10-01

    We have developed a facile and efficient Fe-catalyzed method for fabrication of porous carbons spheres with high graphitization degree (GNPCs) using glucose as carbon precursor at relatively low carbonization temperature. GNPCs not only have relatively large accessible ion surface area to accommodate greater capacity but also high graphitization degree to accelerate ion diffusion. As a typical application, we demonstrate that GNPCs exhibit excellent electrochemical performance for use in supercapacitors, with high specific capacity of 150.6 F g-1 at current density of 1 A g-1 and good rate capability and superior cycling stability over 10,000 cycles, confirming their potential application for energy storage. Moreover, it is believed that this method offers a new strategy for synthesis of porous carbons with high graphitization degree.

  8. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian

    2013-06-01

    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

  9. On-Surface Pseudo-High-Dilution Synthesis of Macrocycles: Principle and Mechanism.

    Science.gov (United States)

    Fan, Qitang; Wang, Tao; Dai, Jingya; Kuttner, Julian; Hilt, Gerhard; Gottfried, J Michael; Zhu, Junfa

    2017-05-23

    Macrocycles have attracted much attention due to their specific "endless" topology, which results in extraordinary properties compared to related linear (open-chain) molecules. However, challenges still remain in their controlled synthesis with well-defined constitution and geometry. Here, we report the successful application of the (pseudo-)high-dilution method to the conditions of on-surface synthesis in ultrahigh vacuum. This approach leads to high yields (up to 84%) of cyclic hyperbenzene ([18]-honeycombene) via an Ullmann-type reaction from 4,4″-dibromo-meta-terphenyl (DMTP) as precursor on a Ag(111) surface. The mechanism of macrocycle formation was explored in detail using scanning tunneling microscopy and X-ray photoemission spectroscopy. We propose that the dominant pathway for hyperbenzene (MTP) 6 formation is the stepwise desilverization of an organometallic (MTP-Ag) 6 macrocycle, which forms via cyclization of (MTP-Ag) 6 chains under pseudo-high-dilution conditions. The high probability of cyclization on the stage of the organometallic phase results from the reversibility of the C-Ag bond. The case is different from that in solution, in which cyclization typically occurs on the stage of a covalently bonded open-chain precursor. This difference in the cyclization mechanism on a surface compared to that in solution stems mainly from the 2D confinement exerted by the surface template, which hinders the flipping of chain segments necessary for cyclization.

  10. Evaluation of the FIR Example using Xilinx Vivado High-Level Synthesis Compiler

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Zheming [Argonne National Lab. (ANL), Argonne, IL (United States); Finkel, Hal [Argonne National Lab. (ANL), Argonne, IL (United States); Yoshii, Kazutomo [Argonne National Lab. (ANL), Argonne, IL (United States); Cappello, Franck [Argonne National Lab. (ANL), Argonne, IL (United States)

    2017-07-28

    Compared to central processing units (CPUs) and graphics processing units (GPUs), field programmable gate arrays (FPGAs) have major advantages in reconfigurability and performance achieved per watt. This development flow has been augmented with high-level synthesis (HLS) flow that can convert programs written in a high-level programming language to Hardware Description Language (HDL). Using high-level programming languages such as C, C++, and OpenCL for FPGA-based development could allow software developers, who have little FPGA knowledge, to take advantage of the FPGA-based application acceleration. This improves developer productivity and makes the FPGA-based acceleration accessible to hardware and software developers. Xilinx Vivado HLS compiler is a high-level synthesis tool that enables C, C++ and System C specification to be directly targeted into Xilinx FPGAs without the need to create RTL manually. The white paper [1] published recently by Xilinx uses a finite impulse response (FIR) example to demonstrate the variable-precision features in the Vivado HLS compiler and the resource and power benefits of converting floating point to fixed point for a design. To get a better understanding of variable-precision features in terms of resource usage and performance, this report presents the experimental results of evaluating the FIR example using Vivado HLS 2017.1 and a Kintex Ultrascale FPGA. In addition, we evaluated the half-precision floating-point data type against the double-precision and single-precision data type and present the detailed results.

  11. Synthesis and reforming of high molecular-weigth compounds by the utilization of radiation

    International Nuclear Information System (INIS)

    Machi, Sueo

    1976-01-01

    Radiation effects on the synthesis are reforming of high molecular-weight compounds are reviewed. The report is divided into four main parts. The first part deals with the characteristics of the radiation processing. The reaction can be started in a wide range of temperature including very low temperature. Catalysts are unnecessary. The reaction velocity is fast, and the reaction in solid phase can be started uniformly. And the quality of products is well controllable. The second part deals with the synthesis of high molecular-weight compounds by radiation polymerization. Radical polymerization and ionizing polymerization, gas phase and liquid phase polymerization, the polymerization and copolymerization of fluorine-containing monomers, and solid phase polymerization and low temperature polymerization are included in this part. Attention is directed to the continuous production system for the radiation polymerization of ethylene developed by Japan Atomic Energy Research Institute. The third part deals with the reforming of high molecular-weight compounds by radiation graft polymerization. The combination of backbone polymers and monomers for reforming plastics and fibers, the membranes for reverse osmosis, porous membranes, and ion exchange membranes are included. The fourth part deals with the reforming of high molecular-weight compounds by the cross-linking. Polyethylene, PVC, ethyl acrylate copolymer and the like are included. (Iwakiri, K.)

  12. Synthesis of alumina nano-sheets via supercritical fluid technology with high uranyl adsorptive capacity

    International Nuclear Information System (INIS)

    Jing Yu; Jun Wang; Zhanshuang Li; Qi Liu; Milin Zhang; Hongbin Bai; Caishan Jiao; Jun Wang; Lianhe Liu

    2012-01-01

    Supercritical carbon dioxide is beneficial to the synthesis of superior ultrafine and uniform materials due to its high chemical stability, low viscosity, high diffusivity, and 'zero' surface tension. γ-Alumina nano-sheets were obtained by a simple hydrothermal route in the presence of supercritical carbon dioxide. XRD, FTIR, SEM, TEM and nitrogen sorption isotherm were employed to characterize the samples. Alumina as-prepared has a high specific surface area of up to 200 ± 6 m 2 g -1 , which presents a high adsorption capacity (4.66 ± 0.02 mg g -1 ) for uranyl ions from aqueous solution. Furthermore, the adsorption process was found to be endothermic and spontaneous in nature. (authors)

  13. Synthesis of niobium carbide by a high energy milling technique of powder metallurgy

    International Nuclear Information System (INIS)

    Antonello, Rodrigo Tecchio; Gonzalez, Cezar Henrique; Urtiga Filho, Severino Leopoldino; Araujo Filho, Oscar Olimpio de; Ambrozio Filho, Francisco

    2010-01-01

    The aim of this work is to obtain and characterize the Niobium Carbide (NbC) by a suitable high energy milling technique using a SPEX Mill vibratory type and niobium and carbon (graphite) powders. Since this carbide is scarced in the national market and it's necessary to apply this NbC as a reinforcement in two molybdenum high speed steels (AISI M2 and AISI M3:2) object of another work motivated this research. The powders were submitted to a high energy milling procedure for suitable times and conditions and then were characterized by means of Scanning Electronic Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray diffraction (DRX) techniques. The ball-to-powder weight ratio was 10:1. The analysed samples showed that the high-energy milling is an alternative route of the NbC synthesis. (author)

  14. Synthesis of niobium carbide (NbC) by powder metallurgy high energy milling technique

    International Nuclear Information System (INIS)

    Antonello, Rodrigo Tecchio; Urtiga Filho, Severino Leopoldino; Araujo Filho, Oscar Olimpio de; Ambrozio Filho, Francisco; Gonzalez, Cezar Henrique

    2009-01-01

    The aim of this work is to obtain and characterize the Niobium Carbide (NbC) by a suitable high energy milling technique using a SPEX Mill vibratory type and niobium and carbon (graphite) powders. Since this carbide is scarce in the national market and it's necessary to apply this NbC as a reinforcement in two molybdenum high speed steels (AISI M2 and AISI M3:2) object of another work motivated this research. The powders were submitted to a high energy milling procedure for suitable times and conditions and then were characterized by means of Scanning Electronic Microscopy (SEM) and X-ray diffraction (DRX) techniques. The ball-to-powder weight ratio was 10:1. The analysed samples showed that the high-energy milling is an alternative route of the NbC synthesis. (author)

  15. Synthesis of Zeolite NaA from Low Grade (High Impurities) Indonesian Natural Zeolite

    OpenAIRE

    Mustain, Asalil; Wibawa, Gede; Nais, Mukhammad Furoiddun; Falah, Miftakhul

    2014-01-01

    The zeolite NaA has been successfully synthesized from the low grade natural zeolite with high impurities. The synthesis method was started by mixing natural zeolite powder with NH4Cl aqueous solution in the reactor as pretreatment. The use of pretreatment was to reduce the impurities contents in the zeolite. The process was followed by alkaline fusion hydrothermal treatment to modify the framework structure of natural zeolite and reduce the SiO2/Al2O3 ratio. Finally, the synthesized zeolite ...

  16. Power Constrained High-Level Synthesis of Battery Powered Digital Systems

    DEFF Research Database (Denmark)

    Nielsen, Sune Fallgaard; Madsen, Jan

    2003-01-01

    We present a high-level synthesis algorithm solving the combined scheduling, allocation and binding problem minimizing area under both latency and maximum power per clock-cycle constraints. Our approach eliminates the large power spikes, resulting in an increased battery lifetime, a property...... of utmost importance for battery powered embedded systems. Our approach extends the partial-clique partitioning algorithm by introducing power awareness through a heuristic algorithm which bounds the design space to those of power feasible schedules. We have applied our algorithm on a set of dataflow graphs...

  17. Ru-assisted synthesis of Pd/Ru nanodendrites with high activity for ethanol electrooxidation

    Science.gov (United States)

    Zhang, Ke; Bin, Duan; Yang, Beibei; Wang, Caiqin; Ren, Fangfang; Du, Yukou

    2015-07-01

    Due to the specific physical and chemical properties of a highly branched noble metal, the controllable synthesis has attracted much attention. This article reports the synthesis of Pd/Ru nanodendrites by a facile method using an oil bath in the presence of polyvinyl pyrrolidone, potassium bromide and ascorbic acid. The morphology, structure, and composition of the as-prepared catalysts were characterized by means of X-ray diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. In the electrochemical measurement, the as-prepared Pd7/Ru1 bimetallic nanodendrites provide a large electrochemically active surface area and exhibit high peak current density in the forward scan toward ethanol electrooxidation, which is nearly four times higher than those of a pure Pd catalyst. The as-prepared Pd7/Ru1 catalysts also exhibit significantly enhanced cycling stability toward ethanol oxidation in alkaline medium, which are mainly ascribed to the synergetic effect between Pd and Ru. This indicates that the Pd7/Ru1 catalysts should have great potential applications in direct ethanol fuel cells.Due to the specific physical and chemical properties of a highly branched noble metal, the controllable synthesis has attracted much attention. This article reports the synthesis of Pd/Ru nanodendrites by a facile method using an oil bath in the presence of polyvinyl pyrrolidone, potassium bromide and ascorbic acid. The morphology, structure, and composition of the as-prepared catalysts were characterized by means of X-ray diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. In the electrochemical measurement, the as-prepared Pd7/Ru1 bimetallic nanodendrites provide a large electrochemically active surface area and exhibit high peak current density in the forward scan toward ethanol electrooxidation, which is nearly four times higher than those of a pure Pd catalyst. The as-prepared Pd7/Ru1 catalysts also exhibit significantly

  18. Template synthesis of highly crystalline and monodisperse iron oxide pigments of nanosize

    International Nuclear Information System (INIS)

    Sreeram, Kalarical Janardhanan; Indumathy, Ramasamy; Rajaram, Ananthanarayanan; Nair, Balachandran Unni; Ramasami, Thirumalachari

    2006-01-01

    Synthesis of highly crystalline and monodisperse iron oxide nanoparticles is reported. The separation of Fe centers through site-specific binding to a polysaccharide-alginate matrix enables the generation of particles with a monodisperse or narrow size distribution character, resulting in transparent pigments. Site-specific interactions coupled with gel like character of alginate is proposed as the mechanism behind generation of lower particle sizes. Alginate-Fe complexes developed were subjected to heat treatment to provide for crystalline character and development of hematite (α-Fe 2 O 3 ). Conditions most ideal for achieving monodispersity and lower sizes have been optimized and confirmed through microscopic and photon correlation spectroscopic measurements

  19. High-performance quantum-dot solids via elemental sulfur synthesis

    KAUST Repository

    Yuan, Mingjian

    2014-03-21

    An elemental-sulfur-based synthesis is reported, which, combined with processing to improve the size dispersion and passivation, results in a low-cost high-quality platform for small-bandgap PbS-CQD-based devices. Size-selective precipitation and cadmium chloride passivation are used to improve the power conversion efficiency of 1 eV bandgap CQD photovoltaic devices dramatically, which leads to record power conversion efficiency for a 1 eV PbS CQD solar cell of 5.4%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Synthesis of high specific activity carbon-11 labeled tracers for neuroreceptor studies

    International Nuclear Information System (INIS)

    Dannals, R.F.; Ravert, H.T.; Wilson, A.A.; Wagner, H.N. Jr; Johns Hopkins Medical Institutions, Baltimore, MD

    1989-01-01

    The use of short-lived positron-emitting radiotracers together with positron emission tomography (PET) has allowed scientists to acquire previously inaccessible information regarding problems in physiology, biochemistry, and pharmacology in the living human body. In the past five years, successes in the application of PET to the non-invasive determination of the spatial distribution and regional concentration of a variety of neurotransmitter binding sites within the living brain often followed the successful selections and syntheses of appropriately radiolabeled ligands. This presentation concentrates on the synthesis of these high specific activity radiotracers for neuroreceptor PET studies labeled specifically with carbon-11. (author). 15 refs.; 1 fig

  1. Rapid Induction of Aldosterone Synthesis in Cultured Neonatal Rat Cardiomyocytes under High Glucose Conditions

    Directory of Open Access Journals (Sweden)

    Masami Fujisaki

    2013-01-01

    Full Text Available In addition to classical adrenal cortical biosynthetic pathway, there is increasing evidence that aldosterone is produced in extra-adrenal tissues. Although we previously reported aldosterone production in the heart, the concept of cardiac aldosterone synthesis remains controversial. This is partly due to lack of established experimental models representing aldosterone synthase (CYP11B2 expression in robustly reproducible fashion. We herein investigated suitable conditions in neonatal rat cardiomyocytes (NRCMs culture system producing CYP11B2 with considerable efficacy. NRCMs were cultured with various glucose doses for 2–24 hours. CYP11B2 mRNA expression and aldosterone concentrations secreted from NRCMs were determined using real-time PCR and enzyme immunoassay, respectively. We found that suitable conditions for CYP11B2 induction included four-hour incubation with high glucose conditions. Under these particular conditions, CYP11B2 expression, in accordance with aldosterone secretion, was significantly increased compared to those observed in the cells cultured under standard-glucose condition. Angiotensin II receptor blocker partially inhibited this CYP11B2 induction, suggesting that there is local renin-angiotensin-aldosterone system activation under high glucose conditions. The suitable conditions for CYP11B2 induction in NRCMs culture system are now clarified: high-glucose conditions with relatively brief period of culture promote CYP11B2 expression in cardiomyocytes. The current system will help to accelerate further progress in research on cardiac tissue aldosterone synthesis.

  2. Synthesis of molecules of biological interest labelled with high specific activity tritium

    International Nuclear Information System (INIS)

    Petillot, Yves

    1975-01-01

    Labelled molecules are artificial organic compounds possessing one or several radioactive or steady isotopic atoms. Using tritium to label molecules presents several benefits: a raw material easy to obtain with a high purity and at reasonable cost; synthesised labelled molecules displaying high specific activities very interesting in molecular biology; high resolution of radiographies; relatively simple and quick introduction of tritium atoms in complex molecules. Thus, this report for graduation in organic chemistry addresses the synthesis and study of new labelled molecules which belong to families of organic compounds which have fundamental activities in biology: uridine 3 H-5,6 and thymidine 3 H-methyl which are nucleotides which intervene under the form of phosphates in the synthesis of nucleic acids, oestradiol 3 H-2,4,6,7 which is a powerful estrogenic hormone which naturally secreted by the ovary; and noradrenaline 3 H-1,1' and dopamine 3 H-1,2 which are usually secreted by adrenal medulla and have multiple actions on the nervous system

  3. Spray-combustion synthesis: efficient solution route to high-performance oxide transistors.

    Science.gov (United States)

    Yu, Xinge; Smith, Jeremy; Zhou, Nanjia; Zeng, Li; Guo, Peijun; Xia, Yu; Alvarez, Ana; Aghion, Stefano; Lin, Hui; Yu, Junsheng; Chang, Robert P H; Bedzyk, Michael J; Ferragut, Rafael; Marks, Tobin J; Facchetti, Antonio

    2015-03-17

    Metal-oxide (MO) semiconductors have emerged as enabling materials for next generation thin-film electronics owing to their high carrier mobilities, even in the amorphous state, large-area uniformity, low cost, and optical transparency, which are applicable to flat-panel displays, flexible circuitry, and photovoltaic cells. Impressive progress in solution-processed MO electronics has been achieved using methodologies such as sol gel, deep-UV irradiation, preformed nanostructures, and combustion synthesis. Nevertheless, because of incomplete lattice condensation and film densification, high-quality solution-processed MO films having technologically relevant thicknesses achievable in a single step have yet to be shown. Here, we report a low-temperature, thickness-controlled coating process to create high-performance, solution-processed MO electronics: spray-combustion synthesis (SCS). We also report for the first time, to our knowledge, indium-gallium-zinc-oxide (IGZO) transistors having densification, nanoporosity, electron mobility, trap densities, bias stability, and film transport approaching those of sputtered films and compatible with conventional fabrication (FAB) operations.

  4. High-yield Synthesis of Multiwalled Carbon Nanotube by Mechanothermal Method

    Directory of Open Access Journals (Sweden)

    Manafi SA

    2009-01-01

    Full Text Available Abstract This study reports on the mechanothermal synthesis of multiwalled carbon nanotube (MWCNTs from elemental graphite powder. Initially, high ultra-active graphite powder can be obtained by mechanical milling under argon atmosphere. Finally, the mechanical activation product is heat-treated at 1350°C for 2–4 h under argon gas flow. After heat-treatment, active graphite powders were successfully changed into MWCNTs with high purity. The XRD analyses showed that in the duration 150 h of milling, all the raw materials were changed to the desired materials. From the broadening of the diffraction lines in the XRD patterns, it was concluded that the graphite crystallites were nanosized, and raising the milling duration resulted in the fineness of the particles and the increase of the strain. The structure and morphology of MWCNTs were investigated using scanning electron microscopy (SEM and high-resolution transmission electron microscopy (HRTEM. The yield of MWCNTs was estimated through SEM and TEM observations of the as-prepared samples was to be about 90%. Indeed, mechanothermal method is of interest for fundamental understanding and improvement of commercial synthesis of carbon nanotubes (CNTs. As a matter of fact, the method of mechanothermal guarantees the production of MWCNTs suitable for different applications.

  5. The direct oxidative diene cyclization and related reactions in natural product synthesis

    Directory of Open Access Journals (Sweden)

    Juliane Adrian

    2016-09-01

    Full Text Available The direct oxidative cyclization of 1,5-dienes is a valuable synthetic method for the (diastereoselective preparation of substituted tetrahydrofurans. Closely related reactions start from 5,6-dihydroxy or 5-hydroxyalkenes to generate similar products in a mechanistically analogous manner. After a brief overview on the history of this group of transformations and a survey on mechanistic and stereochemical aspects, this review article provides a summary on applications in natural product synthesis. Moreover, current limitations and future directions in this area of chemistry are discussed.

  6. New Synthesis and Tritium Labeling of a Selective Ligand for Studying High-affinity γ-Hydroxybutyrate (GHB) Binding Sites

    Science.gov (United States)

    Vogensen, Stine B.; Marek, Aleš; Bay, Tina; Wellendorph, Petrine; Kehler, Jan; Bundgaard, Christoffer; Frølund, Bente; Pedersen, Martin H.F.; Clausen, Rasmus P.

    2013-01-01

    3-Hydroxycyclopent-1-enecarboxylic acid (HOCPCA, 1) is a potent ligand for the high-affinity GHB binding sites in the CNS. An improved synthesis of 1 together with a very efficient synthesis of [3H]-1 is described. The radiosynthesis employs in situ generated lithium trimethoxyborotritide. Screening of 1 against different CNS targets establishes a high selectivity and we demonstrate in vivo brain penetration. In vitro characterization of [3H]-1 binding shows high specificity to the high-affinity GHB binding sites. PMID:24053696

  7. Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

    Science.gov (United States)

    Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

    2015-08-07

    A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

  8. Approaches for introducing high molecular diversity in scaffolds: fast parallel synthesis of highly substituted 1H-quinolin-4-one libraries.

    Science.gov (United States)

    Kuznetsov, Vladimir; Gorohovsky, Sofia; Levy, Amalia; Meir, Simcha; Shkoulev, Vladimir; Menashe, Naim; Greenwald, Moshe; Aizikovich, Alexander; Ofer, Dror; Byk, Gerardo; Gellerman, Garry

    2004-01-01

    We have developed a two steps strategy for the parallel synthesis of highly diversified quinolin-ones. In the first step we have combined and improved different synthetic methods for generating quinolin-4-ones bearing four different substitutions at specific positions using round bottomed flasks. The synthesis was assessed for a large number of substituted quinolin-4-ones. In the second step, the improved method was adapted to a parallel array synthesis using a 12 positions carrousel as demonstrated for the synthesis of 42-variable quinolin-4-ones. The first combinatorial library set 14(a-x) was obtained with a chemical purity of more than 95% without purification, the second library set 15(a-r), which included two synthetic steps, needed combinatorial purification using an innovative parallel purifier. The proposed approach contributes to a more extensive diversification of molecular scaffolds in general and provides access to highly substituted quinolinones in particular.

  9. Stereoselective synthesis of 5-alkoxycarbonyl-4 alkyl-2-anino-3-cyano-6-methyl-4H-pyranes 3 via asymmetric Michael addition to aceptors-gamma-stereogenics; Sintesis esteroselective de 5-alcoxicarbonil-4-alquil-2-amino-3-ciano-6-metil-4H-piranos via adicion Michael sobre aceptores-gama-esterogenicos

    Energy Technology Data Exchange (ETDEWEB)

    Martinez-Grau, A.; Jimenez, B.; Martin, N.; Seoane, C.; Marco, J.L. [Departamento de Quimica Organica, Facultad de Quimica, Universidad Complutense, Madrid (Spain)

    1994-12-31

    The stereoselective synthesis of 5-alkoxycarbonyl-4-alkyl-2-amino-3-cyano-6-methyl-4H-pyrans 3 via asymmetric Michael addition of malononitrile to gamma-stereogenic alpha-acetylacrylates 2 obtained by Knoevenagel reaction of acetylacetates to quiral alpha-hydroxyaldehydes 1 is described. The resulting 2-amino-4H-pyrans 3 have been obtained in moderate yield and good diastereoselectivity. 15 refs.

  10. Honeycomb supports with high thermal conductivity for the Tischer-Tropsch synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Visconti, C.G.; Rronconi, E.; Groppi, G.; Lietti, L. [Politecnico di Milano (Italy). Dipt. di Energia; Iovane, M.; Rossini, S.; Zennaro, R. [Eni S.p.A., San Donato Milanese (Italy). Div. Exploration and Production

    2011-07-01

    The potential of multitubular reactors loaded with washcoated structured catalysts having highly conductive honeycomb supports is investigated herein in the low temperature Fischer- Tropsch synthesis by means of a theoretical investigation. Simulation results indicate that extruded aluminum honeycomb monoliths, washcoated with a Co-based catalyst, are promising for the application at the industrial scale, in particular when adopting supports with high cell densities and catalysts with high activity. Limited temperature gradients within the reactor are in fact possible even at extreme process conditions, thus leading to interesting volumetric reactor yields with negligible pressure drop. This result is achieved without the need of cofeeding to the reactor large amounts of liquid hydrocarbons to remove the reaction heat, as opposite to existing industrial Fischer-Tropsch packed-bed reactors. (orig.)

  11. Development of Highly Efficient Grafting Technique and Synthesis of Natural Polymer-Based Graft Adsorbent

    Energy Technology Data Exchange (ETDEWEB)

    Ueki, Y; Seko, N; Tamada, M [Japan Atomic Energy Agency, Quantum Beam Science Directorate, Takasaki (Japan)

    2012-09-15

    In the framework of the CRP, Japan has focused on the development of fibrous adsorbents for removal of toxic metal ions and recovery of significant metal ions from industrial wastewater and streaming water. Graft polymerization was carried out by using gamma irradiation facility and electron beam accelerator. Emulsion grafting is a novel topic for synthesis of metal ion adsorbents which are prepared from fibrous trunk polymers such as polyethylene fibre and biodegradable nonwoven fabrics. The emulsion grafting, where monomer micelles are dispersed in water in the presence of surfactant, is a highly efficient and economic grafting technique as compared to general organic solvent system. The resultant cotton-based adsorbent has high adsorption efficiency and high adsorption capacity for Hg, besides, it is biodegradable. Polylactic acid can also be used as a trunk material for the grafting. (author)

  12. Low-protein, high-carbohydrate diet increases glucose uptake and fatty acid synthesis in brown adipose tissue of rats.

    Science.gov (United States)

    Aparecida de França, Suélem; Pavani Dos Santos, Maísa; Nunes Queiroz da Costa, Roger Vinícius; Froelich, Mendalli; Buzelle, Samyra Lopes; Chaves, Valéria Ernestânia; Giordani, Morenna Alana; Pereira, Mayara Peron; Colodel, Edson Moleta; Marlise Balbinotti Andrade, Cláudia; Kawashita, Nair Honda

    2014-04-01

    The aim of this study was to evaluate glucose uptake and the contribution of glucose to fatty acid (FA) synthesis and the glycerol-3-phosphate (G3P) of triacylglycerol synthesis by interscapular brown adipose tissue (IBAT) of low-protein, high-carbohydrate (LPHC) diet-fed rats. LPHC (6% protein; 74% carbohydrate) or control (17% protein; 63% carbohydrate) diets were administered to rats (∼ 100 g) for 15 d. Total FA and G3P synthesis and the synthesis of FA and G3P from glucose were evaluated in vivo by (3)H2O and (14)C-glucose. Sympathetic neural contribution for FA synthesis was evaluated by comparing the synthesis in denervated (7 d before) IBAT with that of the contralateral innervated side. The insulin signaling and β3 adrenergic receptor (β3-AR) contents, as well as others, were determined by Western blot (Student's t test or analysis of variance; P ≤ 0.05). Total FA synthesis in IBAT was 133% higher in the LPHC group and was reduced 85% and 70% by denervation for the LPHC and control groups, respectively. Glucose uptake was 3.5-fold higher in the IBAT of LPHC rats than in that of the control rats, and the contribution of glucose to the total FA synthesis increased by 12% in control rats compared with 18% in LPHC rats. The LPHC diet increased the G3P generation from glucose by 270% and the insulin receptor content and the p-AKT insulin stimulation in IBAT by 120% and reduced the β3-AR content by 50%. The LPHC diet stimulated glucose uptake, both the total rates and the rates derived from glucose-dependent FA and G3P synthesis, by increasing the insulin sensitivity and the sympathetic flux, despite a reduction in the β3-AR content. Copyright © 2014 Elsevier Inc. All rights reserved.

  13. Green synthesis of highly fluorescent carbon quantum dots from sugarcane bagasse pulp

    Energy Technology Data Exchange (ETDEWEB)

    Thambiraj, S. [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); Ravi Shankaran, D., E-mail: dravishankaran@hotmail.com [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); National Centre for Nanoscience and Nanotechnology, University of Madras, Guindy Campus, Chennai, 600 025, Tamil Nadu (India)

    2016-12-30

    Graphical abstract: Schematic representation of CQDs from sugarcane bagasse carbon. - Highlights: • CQDs were synthesised from sugarcane bagasse waste with top down approaches. • Synthesis method is green, simple and efficient process. • CQDs possess high quantum yield, good stability and highly fluorescent in nature. • The morphological and topographical study of CQDs was done by HR-TEM and AFM and was observed that the average size is 4.1 ± 0.17 nm and surface thickness is 5 nm. - Abstract: Carbon quantum dots (CQDs) have great potential due to its advantageous characteristics of highly fluorescent nature and good stability. In this study, we aimed to develop a simple and efficient method for the green synthesis of fluorescent CQDs from sugarcane bagasse, a renewable and sustainable resource. The process involves the top down approach of chemical oxidation followed by exfoliation of sugarcane carbon. The synthesized CQDs was characterized by UV–vis absorption spectroscopy, Spectrofluorophotometry, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, X-ray photon spectroscopy (XPS), Atomic force microscopy (AFM) and High-resolution transmission electron microscopy (HR-TEM). The synthesized CQDs possess stable fluorescent properties, good bio-compatibility and high quantum yield. The CQDs are highly crystalline with longitudinal dimensions of 4.1 ± 0.17 nm with an average roughness of around 5 nm. The XRD and TEM analysis indicates that the synthesized CQDs possess face centred cubic crystal structure. The results suggest that the proposed CQDs could be utilized for bio-sensor, bio-imaging and drug delivery applications.

  14. Room temperature synthesis and high temperature frictional study of silver vanadate nanorods.

    Science.gov (United States)

    Singh, D P; Polychronopoulou, K; Rebholz, C; Aouadi, S M

    2010-08-13

    We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly beta-AgV O(3)) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 microm and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 degrees C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O(3) completely transformed into silver vanadium oxide (Ag(2)V(4)O(11)) and silver with an increase in temperature from RT to 700 degrees C.

  15. Mechanical alloying and self-propagating high-temperature synthesis of stable icosahedral quasicrystals

    International Nuclear Information System (INIS)

    Bokhonov, B.B.

    2008-01-01

    The phase evolution of the mechanically alloyed ternary 63%Al + 25%Cu + 12%Fe and 65%Al + 20%Cu + 15%Fe powder mixtures with milling time has been studied by X-ray diffraction method. It was found that an icosahedral quasicrystalline phase was formed directly during high-energy ball milling of the Al-Cu-Fe mixtures. The X-ray and scanning electron microscopic investigations demonstrated the possibility to use self-propagating high-temperature synthesis (SHS) in combination with preliminary mechanical activation for the synthesis of stable icosahedral quasicrystals. The typical morphology of the Al 63 Cu 25 Fe 12 icosahedral quasicrystals formed in the SHS process is a pentagonal dodecahedron with a size of 3-5 mm. The phase composition of the SHS products depends on the time of preliminary mechanical activation. The content of cubic intermetallic phase in SHS products increases with the time of preliminary mechanical activation of the 63%Al + 25%Cu + 12%Fe powder mixtures

  16. Synthesis of highly fluorescent hydrophobic carbon dots by hot injection method using Paraplast as precursor

    International Nuclear Information System (INIS)

    Talib, Abou; Pandey, Sunil; Thakur, Mukeshchand; Wu, Hui-Fen

    2015-01-01

    We have reported synthesis of bright blue colored hydrophobic carbon dots (hC-dots) using highly pure blend of polymers called Paraplast. We developed a hot injection method for making nearly monodispersed hC-dots with a diameter in a range: 5–30 nm as confirmed by high resolution transmission electron microscopy (HRTEM). The involvement of various functional groups was confirmed by Fourier transform infra-red (FTIR) spectroscopy. These hC-dots were incubated with breast cancer stem cells in order to check the entry as well as biological imaging. The cells were analyzed using epifluorescent microscopy. hC-dots showed concentration dependent cytotoxicity (LD 50 : 50 mg/ml) and could be used for bioimaging even at lower concentration (0.5 mg/ml). hC-dots were found to be versatile agents for peeping inside the cells which could also be used for delivery of water insoluble chemotherapeutic agents to variety of solid tumors. - Highlights: • Synthesis of hydrophobic carbon dots from polymer based Paraplast • Deep blue color under the influence of UV light • Typical optical properties used for biological imaging • Biological imaging of breast cancer stem cells revealing potential of carbon dots

  17. High pressure synthesis and investigations of properties of boron allotropes and boron carbide

    International Nuclear Information System (INIS)

    Chuvashova, Irina

    2017-01-01

    This work aimed at the development of the high-pressure high-temperature (HPHT) synthesis of single crystals of boron allotropes and boron-rich compounds, which could be used further for precise investigations of their structures, properties, and behavior at extreme conditions. To summarize, the present work resulted in the HPHT synthesis of the first previously unknown non-icosahedral boron allotrope ζ-B. This finding confirmed earlier theoretical predictions, which stayed unproven for decades because of experimental challenges which couldn't be overcome until recently. Structural stability of α-B and β-B in the Mbar pressure range and B 13 C 2 up to 68 GPa was experimentally proven. Accurate measurements of the unit cell and B 12 icosahedra volumes of the stoichiometric boron carbide B 13 C 2 as a function of pressure led to conclusion that they undergo a similar reduction upon compression that is typical for covalently bonded solids. Neither 'molecular-like' nor 'inversed molecular-like' solid behavior upon compression was detected that has closed a long-standing scientific dispute. A comparison of the compressional behavior of B 13 C 2 with that of α-B and γ-B allotropes and B 4 C showed that it is determined by the types of bonding involved in the course of compression.

  18. Room temperature synthesis and high temperature frictional study of silver vanadate nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Singh, D P; Aouadi, S M [Department of Physics, Southern Illinois University, Carbondale-62901 (United States); Polychronopoulou, K [Department of Chemistry, University of Cyprus, Nicosia, 1678 (Cyprus); Rebholz, C, E-mail: dineshpsingh@gmail.com, E-mail: saouadi@physics.siu.edu [Department of Mechanical and Manufacturing Engineering, University of Cyprus, Nicosia, 1678 (Cyprus)

    2010-08-13

    We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly {beta}-AgV O{sub 3}) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 {mu}m and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 deg. C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O{sub 3} completely transformed into silver vanadium oxide (Ag{sub 2}V{sub 4}O{sub 11}) and silver with an increase in temperature from RT to 700 deg. C.

  19. Synthesis of high-oxidation Y-Ba-Cu-O phases in superoxygenated thin films

    Science.gov (United States)

    Zhang, H.; Gauquelin, N.; McMahon, C.; Hawthorn, D. G.; Botton, G. A.; Wei, J. Y. T.

    2018-03-01

    It is known that solid-state reaction in high-pressure oxygen can stabilize high-oxidation phases of Y-Ba-Cu-O superconductors in powder form. We extend this superoxygenation concept of synthesis to thin films which, due to their large surface-to-volume ratio, are more reactive thermodynamically. Epitaxial thin films of YBa2Cu3O7 -δ grown by pulsed laser deposition are annealed at up to 700 atm O2 and 900 ∘C , in conjunction with Cu enrichment by solid-state diffusion. The films show the clear formation of Y2Ba4Cu7O15 -δ and Y2Ba4Cu8O16 as well as regions of YBa2Cu5O9 -δ and YBa2Cu6O10 -δ phases, according to scanning transmission electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Similarly annealed YBa2Cu3O7 -δ powders show no phase conversion. Our results demonstrate a route of synthesis towards discovering more complex phases of cuprates and other superconducting oxides.

  20. Multi-exposure high dynamic range image synthesis with camera shake correction

    Science.gov (United States)

    Li, Xudong; Chen, Yongfu; Jiang, Hongzhi; Zhao, Huijie

    2017-10-01

    Machine vision plays an important part in industrial online inspection. Owing to the nonuniform illuminance conditions and variable working distances, the captured image tends to be over-exposed or under-exposed. As a result, when processing the image such as crack inspection, the algorithm complexity and computing time increase. Multiexposure high dynamic range (HDR) image synthesis is used to improve the quality of the captured image, whose dynamic range is limited. Inevitably, camera shake will result in ghost effect, which blurs the synthesis image to some extent. However, existed exposure fusion algorithms assume that the input images are either perfectly aligned or captured in the same scene. These assumptions limit the application. At present, widely used registration based on Scale Invariant Feature Transform (SIFT) is usually time consuming. In order to rapidly obtain a high quality HDR image without ghost effect, we come up with an efficient Low Dynamic Range (LDR) images capturing approach and propose a registration method based on ORiented Brief (ORB) and histogram equalization which can eliminate the illumination differences between the LDR images. The fusion is performed after alignment. The experiment results demonstrate that the proposed method is robust to illumination changes and local geometric distortion. Comparing with other exposure fusion methods, our method is more efficient and can produce HDR images without ghost effect by registering and fusing four multi-exposure images.

  1. InSe monolayer: synthesis, structure and ultra-high second-harmonic generation

    Science.gov (United States)

    Zhou, Jiadong; Shi, Jia; Zeng, Qingsheng; Chen, Yu; Niu, Lin; Liu, Fucai; Yu, Ting; Suenaga, Kazu; Liu, Xinfeng; Lin, Junhao; Liu, Zheng

    2018-04-01

    III–IV layered materials such as indium selenide have excellent photoelectronic properties. However, synthesis of materials in such group, especially with a controlled thickness down to monolayer, still remains challenging. Herein, we demonstrate the successful synthesis of monolayer InSe by physical vapor deposition (PVD) method. The high quality of the sample was confirmed by complementary characterization techniques such as Raman spectroscopy, atomic force microscopy (AFM) and high resolution annular dark field scanning transmission electron microscopy (ADF-STEM). We found the co-existence of different stacking sequence (β- and γ-InSe) in the same flake with a sharp grain boundary in few-layered InSe. Edge reconstruction is also observed in monolayer InSe, which has a distinct atomic structure from the bulk lattice. Moreover, we discovered that the second-harmonic generation (SHG) signal from monolayer InSe shows large optical second-order susceptibility that is 1–2 orders of magnitude higher than MoS2, and even 3 times of the largest value reported in monolayer GaSe. These results make atom-thin InSe a promising candidate for optoelectronic and photosensitive device applications.

  2. Synthesis of highly fluorescent hydrophobic carbon dots by hot injection method using Paraplast as precursor

    Energy Technology Data Exchange (ETDEWEB)

    Talib, Abou [Doctoral Degree Program in Marine Biotechnology, National Sun Yat-Sen University, Kaohsiung 80424, Taiwan (China); Pandey, Sunil [Department of Chemistry, National Sun Yat-Sen University, 70, Lien-Hai Road, Kaohsiung 80424, Taiwan (China); Center for Nanoscience and Nanotechnology, National Sun Yat-Sen University, 70, Lien-Hai Road, Kaohsiung 80424, Taiwan (China); Thakur, Mukeshchand [Department of Chemistry, National Sun Yat-Sen University, 70, Lien-Hai Road, Kaohsiung 80424, Taiwan (China); Wu, Hui-Fen, E-mail: hui@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-Sen University, 70, Lien-Hai Road, Kaohsiung 80424, Taiwan (China); Center for Nanoscience and Nanotechnology, National Sun Yat-Sen University, 70, Lien-Hai Road, Kaohsiung 80424, Taiwan (China); Doctoral Degree Program in Marine Biotechnology, National Sun Yat-Sen University, Kaohsiung 80424, Taiwan (China); School of Pharmacy, College of Pharmacy, Kaohsiung Medical University, Kaohsiung 800, Taiwan (China); Institute of Medical Science and Technology, National Sun Yat-Sen University, Kaohsiung, 80424, Taiwan (China)

    2015-03-01

    We have reported synthesis of bright blue colored hydrophobic carbon dots (hC-dots) using highly pure blend of polymers called Paraplast. We developed a hot injection method for making nearly monodispersed hC-dots with a diameter in a range: 5–30 nm as confirmed by high resolution transmission electron microscopy (HRTEM). The involvement of various functional groups was confirmed by Fourier transform infra-red (FTIR) spectroscopy. These hC-dots were incubated with breast cancer stem cells in order to check the entry as well as biological imaging. The cells were analyzed using epifluorescent microscopy. hC-dots showed concentration dependent cytotoxicity (LD{sub 50}: 50 mg/ml) and could be used for bioimaging even at lower concentration (0.5 mg/ml). hC-dots were found to be versatile agents for peeping inside the cells which could also be used for delivery of water insoluble chemotherapeutic agents to variety of solid tumors. - Highlights: • Synthesis of hydrophobic carbon dots from polymer based Paraplast • Deep blue color under the influence of UV light • Typical optical properties used for biological imaging • Biological imaging of breast cancer stem cells revealing potential of carbon dots.

  3. High pressure synthesis and investigations of properties of boron allotropes and boron carbide

    Energy Technology Data Exchange (ETDEWEB)

    Chuvashova, Irina

    2017-06-12

    This work aimed at the development of the high-pressure high-temperature (HPHT) synthesis of single crystals of boron allotropes and boron-rich compounds, which could be used further for precise investigations of their structures, properties, and behavior at extreme conditions. To summarize, the present work resulted in the HPHT synthesis of the first previously unknown non-icosahedral boron allotrope ζ-B. This finding confirmed earlier theoretical predictions, which stayed unproven for decades because of experimental challenges which couldn't be overcome until recently. Structural stability of α-B and β-B in the Mbar pressure range and B{sub 13}C{sub 2} up to 68 GPa was experimentally proven. Accurate measurements of the unit cell and B{sub 12} icosahedra volumes of the stoichiometric boron carbide B{sub 13}C{sub 2} as a function of pressure led to conclusion that they undergo a similar reduction upon compression that is typical for covalently bonded solids. Neither 'molecular-like' nor 'inversed molecular-like' solid behavior upon compression was detected that has closed a long-standing scientific dispute. A comparison of the compressional behavior of B{sub 13}C{sub 2} with that of α-B and γ-B allotropes and B{sub 4}C showed that it is determined by the types of bonding involved in the course of compression.

  4. Synthesis of multi-wavelength temporal phase-shifting algorithms optimized for high signal-to-noise ratio and high detuning robustness using the frequency transfer function.

    Science.gov (United States)

    Servin, Manuel; Padilla, Moises; Garnica, Guillermo

    2016-05-02

    Synthesis of single-wavelength temporal phase-shifting algorithms (PSA) for interferometry is well-known and firmly based on the frequency transfer function (FTF) paradigm. Here we extend the single-wavelength FTF-theory to dual and multi-wavelength PSA-synthesis when several simultaneous laser-colors are present. The FTF-based synthesis for dual-wavelength (DW) PSA is optimized for high signal-to-noise ratio and minimum number of temporal phase-shifted interferograms. The DW-PSA synthesis herein presented may be used for interferometric contouring of discontinuous industrial objects. Also DW-PSA may be useful for DW shop-testing of deep free-form aspheres. As shown here, using the FTF-based synthesis one may easily find explicit DW-PSA formulae optimized for high signal-to-noise and high detuning robustness. To this date, no general synthesis and analysis for temporal DW-PSAs has been given; only ad hoc DW-PSAs formulas have been reported. Consequently, no explicit formulae for their spectra, their signal-to-noise, their detuning and harmonic robustness has been given. Here for the first time a fully general procedure for designing DW-PSAs (or triple-wavelengths PSAs) with desire spectrum, signal-to-noise ratio and detuning robustness is given. We finally generalize DW-PSA to higher number of wavelength temporal PSAs.

  5. α-Haloaldehydes: versatile building blocks for natural product synthesis.

    Science.gov (United States)

    Britton, Robert; Kang, Baldip

    2013-02-01

    The diastereoselective addition of organometallic reagents to α-chloroaldehydes was first reported in 1959 and occupies a historically significant role as the prototypical reaction for Cornforth's model of stereoinduction. Despite clear synthetic potential for these reagents, difficulties associated with producing enantiomerically enriched α-haloaldehydes limited their use in natural product synthesis through the latter half of the 20th century. In recent years, however, a variety of robust, organocatalytic processes have been reported that now provide direct access to optically enriched α-haloaldehydes and have motivated renewed interest in their use as building blocks for natural product synthesis. This Highlight summarizes the methods available for the enantioselective preparation of α-haloaldehydes and their stereoselective conversion into natural products.

  6. One-step synthesis of dimethyl ether from the gas mixture containing CO2 with high space velocity

    International Nuclear Information System (INIS)

    Chen, Wei-Hsin; Lin, Bo-Jhih; Lee, How-Ming; Huang, Men-Han

    2012-01-01

    Highlights: ► A bifunctional catalyst for DME synthesis is prepared using a coprecipitation method. ► The DME synthesis from syngas at a high space velocity of is investigated. ► The reaction is dominated by chemical kinetics at lower reaction temperatures. ► Thermodynamic equilibrium governs the reaction at higher temperatures. ► 0.2 g of ZSM5 is sufficient to be blended with 1 g of the catalyst for DME synthesis. -- Abstract: Dimethyl ether (DME) has been considered as a potential hydrogen carrier used in fuel cells; it can also be consumed as a diesel substitute or chemicals. To develop the technique of DME synthesis, a bifunctional Cu–ZnO–Al 2 O 3 /ZSM5 catalyst is prepared using a coprecipitation method. The reaction characteristics of DME synthesis from syngas at a high space velocity of 15,000 mL (g cat h) −1 are investigated and the effects of reaction temperature, pressure, CO 2 concentration and ZSM5 amount on the synthesis are taken into account. The results suggest that an increase in CO 2 concentration in the feed gas substantially decreases the DME formation. The optimum reaction temperature always occurs at 225 °C, regardless of what the pressure is. It is thus recognized that the DME synthesis is governed by two different mechanisms when the reaction temperature varies. At lower reaction temperatures ( 225 °C). For the CO 2 content of 5 vol.% and the pressure of 40 atm, the maximum DME yield is 1.89 g (g cat h) −1 . It is also found that 0.2 g of ZSM5 is sufficient to be blended with 1 g of the catalyst for DME synthesis.

  7. Asymmetric synthesis of α-amino acids via homologation of Ni(II) complexes of glycine Schiff bases; Part 1: alkyl halide alkylations.

    Science.gov (United States)

    Sorochinsky, Alexander E; Aceña, José Luis; Moriwaki, Hiroki; Sato, Tatsunori; Soloshonok, Vadim A

    2013-10-01

    Alkylations of chiral or achiral Ni(II) complexes of glycine Schiff bases constitute a landmark in the development of practical methodology for asymmetric synthesis of α-amino acids. Straightforward, easy preparation as well as high reactivity of these Ni(II) complexes render them ready available and inexpensive glycine equivalents for preparing a wide variety of α-amino acids, in particular on a relatively large scale. In the case of Ni(II) complexes containing benzylproline moiety as a chiral auxiliary, their alkylation proceeds with high thermodynamically controlled diastereoselectivity. Similar type of Ni(II) complexes derived from alanine can also be used for alkylation providing convenient access to quaternary, α,α-disubstituted α-amino acids. Achiral type of Ni(II) complexes can be prepared from picolinic acid or via recently developed modular approach using simple secondary or primary amines. These Ni(II) complexes can be easily mono/bis-alkylated under homogeneous or phase-transfer catalysis conditions. Origin of diastereo-/enantioselectivity in the alkylations reactions, aspects of practicality, generality and limitations of this methodology is critically discussed.

  8. High-gravity combustion synthesis and in situ melt infiltration: A new method for preparing cemented carbides

    International Nuclear Information System (INIS)

    Liu, Guanghua; Li, Jiangtao; Yang, Zengchao; Guo, Shibin; Chen, Yixiang

    2013-01-01

    A new method of high-gravity combustion synthesis and in situ melt infiltration is reported for preparing cemented carbides, where hot nickel melt is in situ synthesized from a highly exothermic combustion reaction and then infiltrated into tungsten carbide powder compacts. The as-prepared sample showed a homogeneous microstructure, and its relative density, hardness and flexural strength were 94.4%, 84 HRA and 1.49 GPa, respectively. Compared with conventional powder metallurgy approaches, high-gravity combustion synthesis offers a fast and furnace-free way to produce cemented carbides

  9. High-rate synthesis of microcrystalline silicon films using high-density SiH4/H2 microwave plasma

    International Nuclear Information System (INIS)

    Jia, Haijun; Saha, Jhantu K.; Ohse, Naoyuki; Shirai, Hajime

    2007-01-01

    A high electron density (> 10 11 cm -3 ) and low electron temperature (1-2 eV) plasma is produced by using a microwave plasma source utilizing a spoke antenna, and is applied for the high-rate synthesis of high quality microcrystalline silicon (μc-Si) films. A very fast deposition rate of ∼ 65 A/s is achieved at a substrate temperature of 150 deg. C with a high Raman crystallinity and a low defect density of (1-2) x 10 16 cm -3 . Optical emission spectroscopy measurements reveal that emission intensity of SiH and intensity ratio of H α /SiH are good monitors for film deposition rate and film crystallinity, respectively. A high flux of film deposition precursor and atomic hydrogen under a moderate substrate temperature condition is effective for the fast deposition of highly crystallized μc-Si films without creating additional defects as well as for the improvement of film homogeneity

  10. Optimization of components in high-yield synthesis of block copolymer-mediated gold nanoparticles

    International Nuclear Information System (INIS)

    Ray, Debes; Aswal, Vinod Kumar

    2012-01-01

    The optimization to achieve stable and high-yield gold nanoparticles in block copolymer-mediated synthesis has been examined. Gold nanoparticles are synthesized using block copolymer P85 in gold salt HAuCl 4 ·3H 2 O solution. This method usually has a very limited yield which does not simply increase with the increase in the gold salt concentration. We show that the yield can be enhanced by increasing the block copolymer concentration but is limited to the factor by which the concentration is increased. On the other hand, the presence of an additional reductant (trisodium citrate) in 1:1 molar ratio with gold salt enhances the yield by manyfold. In this case (with additional reductant), the stable and high-yield nanoparticles having size about 14 nm can be synthesized at very low block copolymer concentrations. These nanoparticles thus can be efficiently used for their application such as for adsorption of proteins.

  11. Synthesis and characterization of high performance superabsorbent hydrogels using bis[2-(methacryloyloxyethyl] phosphate as crosslinker

    Directory of Open Access Journals (Sweden)

    A. A. L. Goncalves

    2016-03-01

    Full Text Available Various superabsorbent polymers (SAPs were synthesized by free radical copolymerization at 70°C using acrylic acid (AA, potassium acrylate (KA, N-isopropyl acrylamide (NIPAM and sulfopropyl methacrylate potassium salt (SPM as monomers, bis[2-(methacryloyloxyethyl] phosphate (BMEP as crosslinker and potassium persulfate (KPS as initiator. The optimization of the synthesis led to the preparation of a SAP with very high water absorption ability, with a maximum swelling of 2618 g water/g dry hydrogel. The most promising SAP was fully characterized and the absorption capacities were studied at different pH and ionic strengths. When this SAP was mixed with soil, the mixture was able to lose water more slowly. Also, this material revealed high loading capacity and showed good releasing profiles using urea as model fertilizer. Due to these advantageous properties, the synthesized SAP can be used in agricultural applications.

  12. Highly Efficient Synthesis of 2-Aryl-3-methoxyacrylates via Suzuki-Miyaura Coupling Reaction

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hyung Ho; Lee, Chun Ho; Song, Young Seob; Park, No Kyun; Kim, Bum Tae; Heo, Jung Nyoung [Korea Research Institute of Chemical Technology, Daejeon (Korea, Republic of)

    2006-02-15

    We have developed a highly efficient and convergent synthesis of 2-aryl-3-methoxyacrylates via the Suzuki-Miyaura coupling reaction of α-iodo-β-methoxy-acrylate with arylboronic acids. The biological activities of 2-aryl-3-methoxyacrylate derivatives will be reported in due course. The Suzuki-Miyaura coupling reaction provides a convenient access to the carbon-carbon bond formation with high efficiency. Recently, a number of 2-aryl-3-methoxy-acrylates served as a key scaffold for the development of biologically active pharmaceuticals and agrochemicals. Especially, the discovery of the naturally-occurring fungicides, such as strobilurin A and oudemansin A, possessing a β-methoxyacrylate moiety was immediately seized great attention by industrial research groups to open a new era of the strobilurin family including azoxy-strobin and picoxystrobin.

  13. Synthesis and characterization of DC magnetron sputtered ZnO thin films under high working pressures

    International Nuclear Information System (INIS)

    Hezam, M.; Tabet, N.; Mekki, A.

    2010-01-01

    ZnO thin films were deposited on glass substrates using direct current (dc) magnetron sputtering under high working pressures. A pure zinc target was used, and sputtering was carried out in an oxygen atmosphere. The working pressure was varied between 50 and 800 mTorr. XRD characterization showed that for a window of working pressures between 300 and 500 mTorr, the deposited films were polycrystalline, with strong preferential orientation of grains along the c-axis. The film deposited at 400 mTorr had the highest (002) peak with the largest estimated grain size. Outside this window, the crystallinity and c-orientation of grains are lost. The microstructure of the films was investigated by Atomic Force microscopy (AFM). Optical transparency of the films was about 85%. The films produced were highly resistive, which might provide new alternatives for the synthesis of ZnO thin films aimed for SAW devices.

  14. Robust image registration for multiple exposure high dynamic range image synthesis

    Science.gov (United States)

    Yao, Susu

    2011-03-01

    Image registration is an important preprocessing technique in high dynamic range (HDR) image synthesis. This paper proposed a robust image registration method for aligning a group of low dynamic range images (LDR) that are captured with different exposure times. Illumination change and photometric distortion between two images would result in inaccurate registration. We propose to transform intensity image data into phase congruency to eliminate the effect of the changes in image brightness and use phase cross correlation in the Fourier transform domain to perform image registration. Considering the presence of non-overlapped regions due to photometric distortion, evolutionary programming is applied to search for the accurate translation parameters so that the accuracy of registration is able to be achieved at a hundredth of a pixel level. The proposed algorithm works well for under and over-exposed image registration. It has been applied to align LDR images for synthesizing high quality HDR images..

  15. Synthesis and Characterization of High-Dielectric-Constant Nanographite-Polyurethane Composite

    Science.gov (United States)

    Mishra, Praveen; Bhat, Badekai Ramachandra; Bhattacharya, B.; Mehra, R. M.

    2018-05-01

    In the face of ever-growing demand for capacitors and energy storage devices, development of high-dielectric-constant materials is of paramount importance. Among various dielectric materials available, polymer dielectrics are preferred for their good processability. We report herein synthesis and characterization of nanographite-polyurethane composite with high dielectric constant. Nanographite showed good dispersibility in the polyurethane matrix. The thermosetting nature of polyurethane gives the composite the ability to withstand higher temperature without melting. The resultant composite was studied for its dielectric constant (ɛ) as a function of frequency. The composite exhibited logarithmic variation of ɛ from 3000 at 100 Hz to 225 at 60 kHz. The material also exhibited stable dissipation factor (tan δ) across the applied frequencies, suggesting its ability to resist current leakage.

  16. Highly Stereoselective Synthesis of Cyclopentanes bearing Four Stereocenters by a Rhodium Carbene–Initiated Domino Sequence

    Science.gov (United States)

    Parr, Brendan T.; Davies, Huw M. L.

    2014-01-01

    Stereoselective synthesis of a cyclopentane nucleus by convergent annulations constitutes a significant challenge for synthetic chemists. Though a number of biologically relevant cyclopentane natural products are known, more often than not, the cyclopentane core is assembled in a stepwise fashion due to lack of efficient annulation strategies. Herein, we report the rhodium-catalyzed reactions of vinyldiazoacetates with (E)-1,3-disubstituted 2-butenols generate cyclopentanes, containing four new stereogenic centers with very high levels of stereoselectivity (99% ee, >97 : 3 dr). The reaction proceeds by a carbene–initiated domino sequence consisting of five distinct steps: rhodium–bound oxonium ylide formation, [2,3]-sigmatropic rearrangement, oxy-Cope rearrangement, enol–keto tautomerization, and finally an intramolecular carbonyl ene reaction. A systematic study is presented detailing how to control chirality transfer in each of the four stereo-defining steps of the cascade, consummating in the development of a highly stereoselective process. PMID:25082301

  17. Polar-solvent-free colloidal synthesis of highly luminescent alkylammonium lead halide perovskite nanocrystals

    Science.gov (United States)

    Vybornyi, Oleh; Yakunin, Sergii; Kovalenko, Maksym V.

    2016-03-01

    A novel synthesis of hybrid organic-inorganic lead halide perovskite nanocrystals (CH3NH3PbX3, X = Br or I) that does not involve the use of dimethylformamide or other polar solvents is presented. The reaction between methylamine and PbX2 salts is conducted in a high-boiling nonpolar solvent (1-octadecene) in the presence of oleylamine and oleic acid as coordinating ligands. The resulting nanocrystals are characterized by high photoluminescence quantum efficiencies of 15-50%, outstanding phase purity and tunable shapes (nanocubes, nanowires, and nanoplatelets). Nanoplatelets spontaneously assemble into micrometer-length wires by face-to-face stacking. In addition, we demonstrate amplified spontaneous emission from thin films of green-emitting CH3NH3PbBr3 nanowires with low pumping thresholds of 3 μJ cm-2.A novel synthesis of hybrid organic-inorganic lead halide perovskite nanocrystals (CH3NH3PbX3, X = Br or I) that does not involve the use of dimethylformamide or other polar solvents is presented. The reaction between methylamine and PbX2 salts is conducted in a high-boiling nonpolar solvent (1-octadecene) in the presence of oleylamine and oleic acid as coordinating ligands. The resulting nanocrystals are characterized by high photoluminescence quantum efficiencies of 15-50%, outstanding phase purity and tunable shapes (nanocubes, nanowires, and nanoplatelets). Nanoplatelets spontaneously assemble into micrometer-length wires by face-to-face stacking. In addition, we demonstrate amplified spontaneous emission from thin films of green-emitting CH3NH3PbBr3 nanowires with low pumping thresholds of 3 μJ cm-2. Electronic supplementary information (ESI) available: Materials and methods, additional figures. See DOI: 10.1039/c5nr06890h

  18. Synthesis of high-quality mesoporous silicon particles for enhanced lithium storage performance

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chundong, E-mail: apcdwang@hust.edu.cn [School of Optical and Electronic Information, Huazhong University of Science and Technology, Wuhan 430074 (China); Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Ren, Jianguo [Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Chen, Hao [Department of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou (China); Zhang, Yi [School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan, 430073 (China); Ostrikov, Kostya [School of Chemistry, Physics, and Mechanical Engineering, Queensland University of Technology, Brisbane 4000, QLD (Australia); Manufacturing Flagship, CSIRO, P. O. Box 218, Lindfield, NSW 2070 (Australia); Zhang, Wenjun [Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China); Li, Yi, E-mail: liyi@suda.edu.cn [Department of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou (China); Center of Super-Diamond and Advanced Films (COSDAF), Department of Physics and Materials Science, City University of Hong Kong, Kowloon, Hong Kong SAR (China)

    2016-04-15

    Silicon has been considered as one of the most promising anode materials for high-capacity lithium-ion batteries (LIBs) due to its ultrahigh theoretical capacity, abundance, and environmentally benign nature. Nonetheless, the severe break during the prolonged cycling results in poor electrochemical performance, which hinders its practical application. Herein, we report the synthesis of novel mesoporous silicon particles with a facile template method by using a magnesiothermic reduction for LIBs. The obtained silicon nanoparticles are highly porous with densely porous cavities (20–40 nm) on the wall, of which it presents good crystallization. Electrochemical measurements showed that the mesoporous silicon nanoparticles delivered a high reversible specific capacity of 910 mA h g{sup −1} at a high current density of 1200 mA g{sup −1} over 50 cycles. The specific capacity at such high current density is still over twofold than that of commercial graphite anode, suggesting that the nanoporous Si architectures is suitable for high-performance Si-based anodes for lithium ion batteries in terms of capacity, cycle life, and rate capacity. - Highlights: • Silica nanotubes were prepared with a facile template method. • Novel mesoporous silicon particles were obtained by magnesiothermic reduction. • High-Performance LIBs were achieved by using mesoporous Si particle Electrodes.

  19. Carbon Isotope Systematics in Mineral-Catalyzed Hydrothermal Organic Synthesis Processes at High Temperature and Pressures

    Science.gov (United States)

    Fu, Qi; Socki, R. A.; Niles, Paul B.

    2011-01-01

    Observation of methane in the Martian atmosphere has been reported by different detection techniques. Reduction of CO2 and/or CO during serpentization by mineral surface catalyzed Fischer-Tropsch Type (FTT) synthesis may be one possible process responsible for methane generation on Mars. With the evidence a recent study has discovered for serpentinization in deeply buried carbon rich sediments, and more showing extensive water-rock interaction in Martian history, it seems likely that abiotic methane generation via serpentinization reactions may have been common on Mars. Experiments involving mineral-catalyzed hydrothermal organic synthesis processes were conducted at 750 C and 5.5 Kbars. Alkanes, alcohols and carboxylic acids were identified as organic compounds. No "isotopic reversal" of delta C-13 values was observed for alkanes or carboxylic acids, suggesting a different reaction pathway than polymerization. Alcohols were proposed as intermediaries formed on mineral surfaces at experimental conditions. Carbon isotope data were used in this study to unravel the reaction pathways of abiotic formation of organic compounds in hydrothermal systems at high temperatures and pressures. They are instrumental in constraining the origin and evolution history of organic compounds on Mars and other planets.

  20. High-Level Synthesis of DSP Applications Using Adaptive Negative Cycle Detection

    Directory of Open Access Journals (Sweden)

    Nitin Chandrachoodan

    2002-09-01

    Full Text Available The problem of detecting negative weight cycles in a graph is examined in the context of the dynamic graph structures that arise in the process of high level synthesis (HLS. The concept of adaptive negative cycle detection is introduced, in which a graph changes over time and negative cycle detection needs to be done periodically, but not necessarily after every individual change. We present an algorithm for this problem, based on a novel extension of the well-known Bellman-Ford algorithm that allows us to adapt existing cycle information to the modified graph, and show by experiments that our algorithm significantly outperforms previous incremental approaches for dynamic graphs. In terms of applications, the adaptive technique leads to a very fast implementation of Lawlers algorithm for the computation of the maximum cycle mean (MCM of a graph, especially for a certain form of sparse graph. Such sparseness often occurs in practical circuits and systems, as demonstrated, for example, by the ISCAS 89/93 benchmarks. The application of the adaptive technique to design-space exploration (synthesis is also demonstrated by developing automated search techniques for scheduling iterative data-flow graphs.

  1. Sample preparation of environmental samples using benzene synthesis followed by high-performance LSC

    International Nuclear Information System (INIS)

    Filippis, S. De; Noakes, J.E.

    1991-01-01

    Liquid scintillation counting (LSC) techniques have been widely employed as the detection method for determining environmental levels of tritium and 14 C. Since anthropogenic and nonanthropogenic inputs to the environment are a concern, sampling the environment surrounding a nuclear power facility or fuel reprocessing operation requires the collection of many different sample types, including agriculture products, water, biota, aquatic life, soil, and vegetation. These sample types are not suitable for the direct detection of tritium of 14 C for liquid scintillation techniques. Each sample type must be initially prepared in order to obtain the carbon or hydrogen component of interest and present this in a chemical form that is compatible with common chemicals used in scintillation counting applications. Converting the sample of interest to chemically pure benzene as a sample preparation technique has been widely accepted for processing samples for radiocarbon age-dating applications. The synthesized benzene is composed of the carbon or hydrogen atoms from the original sample and is ideal as a solvent for LSC with excellent photo-optical properties. Benzene synthesis followed by low-background scintillation counting can be applied to the preparation and measurement of environmental samples yielding good detection sensitivities, high radionuclide counting efficiency, and shorter preparation time. The method of benzene synthesis provides a unique approach to the preparation of a wide variety of environmental sample types using similar chemistry for all samples

  2. Synthesis of belt-like BiOBr hierarchical nanostructure with high photocatalytic performance

    Energy Technology Data Exchange (ETDEWEB)

    Li, Haiping [National Engineering Technology Research Center for Colloidal Materials, Shandong University, Jinan 250100 (China); Liu, Jingyi; Hu, Tingxia [Environment Research Institute, Shandong University, Jinan 250100 (China); Du, Na; Song, Shue [Key Laboratory of Colloid and Interface Chemistry (Ministry of Education), Shandong University, Jinan 250100 (China); Hou, Wanguo, E-mail: wghou@sdu.edu.cn [Key Laboratory of Colloid and Interface Chemistry (Ministry of Education), Shandong University, Jinan 250100 (China)

    2016-05-15

    Highlights: • BiOBr hierarchical nanobelts (NBs) were solvothermally prepared. • NBs show higher specific surface area and photoabsorption than BiOBr nanosheets. • NBs exhibit higher photoactivity than the nanosheets. - Abstract: One-dimensional (1D) bismuth oxyhalide (BiOX) hierarchical nanostructures are always difficult to prepare. Herein, we report, for the first time, a simple synthesis of BiOBr nanobelts (NBs) via a facile solvothermal route, using bismuth subsalicylate as the template and bismuth source. The BiOBr nanobelts are composed of irregular single crystal nanoparticles with highly exposed (0 1 0) facets. Compared with the BiOBr nanosheets (NSs) with dominant exposed (0 0 1) facets, they exhibit higher photocatalytic activity toward degradation of Rhodamine B and Methylene Blue under visible light irradiation. The higher photocatalytic performance of BiOBr NBs arises from their larger specific surface area and higher photoabsorption capability. This study provides a simple route for synthesis of belt-like Bi-based hierarchical nanostructures.

  3. Minute-made and low carbon fingerprint microwave synthesis of high quality templated mesoporous silica

    KAUST Repository

    Chaignon, J.; Bouizi, Y.; Davin, L.; Calin, N.; Albela, B.; Bonneviot, L.

    2015-01-01

    © The Royal Society of Chemistry 2015. Hexagonal mesostructured templated silicas were produced in less than 10 minutes using an ultra-fast microwave assisted hydrothermal synthesis. Typically, 10 g can be prepared at once in a commercial microwave device usually devoted to analytical digestion. Undesired alcohol side-products were avoided using inexpensive water colloidal silica instead of silicon alkoxides as the silicon source. In comparison with classical heating activation, the absence of pore expansion and pore wall thickening even for synthesis temperatures as high as 190 °C evidenced that heat transfer and diffusion of matter had no time to take place. Comparison between the chemically extracted and calcined samples shows that the structure was better stabilized for autoclaving above 150 °C. However, a fast temperature ramping and final temperatures above 180 °C were required to sear structures of the highest quality comparable to that of the best conventional methods. This is rationalized by assuming a sequential flake-by-flake assembly of the pore-wall at the micelle palisade. Notably, tosylate counterions yielded better structural characteristics than bromide counterions and allowed better opportunities for surfactant recycling.

  4. High Pressure Diels Alder Reactions of 1-Vinyl-2,2,6-trimethylcyclohexene Catalyzed by Chiral Lewis Acids; An Enantioselective Route to a Drimane Sesquiterpene Precursor.

    NARCIS (Netherlands)

    Knol, Joop; Meetsma, Auke; Feringa, Bernard

    1995-01-01

    The Diels Alder reaction of 1-vinyl-2,2,6-trimethylcyclohexene and 3-((E)-3-(methoxycarbonyl)propenoyl)-1,3-oxazolidin-2-one under high pressure, catalyzed by a chiral bis-imine copper(II) complex, yields a drimane sesquiterpene precursor in a highly regio- and diastereoselective manner with

  5. A template-free solvent-mediated synthesis of high surface area boron nitride nanosheets for aerobic oxidative desulfurization.

    Science.gov (United States)

    Wu, Peiwen; Zhu, Wenshuai; Chao, Yanhong; Zhang, Jinshui; Zhang, Pengfei; Zhu, Huiyuan; Li, Changfeng; Chen, Zhigang; Li, Huaming; Dai, Sheng

    2016-01-04

    Hexagonal boron nitride nanosheets (h-BNNs) with rather high specific surface area (SSA) are important two-dimensional layer-structured materials. Here, a solvent-mediated synthesis of h-BNNs revealed a template-free lattice plane control strategy that induced high SSA nanoporous structured h-BNNs with outstanding aerobic oxidative desulfurization performance.

  6. Thermodynamically Controlled High-Pressure High-Temperature Synthesis of Crystalline Fluorinated sp 3 -Carbon Networks

    Energy Technology Data Exchange (ETDEWEB)

    Klier, Kamil; Landskron, Kai

    2015-11-19

    We report the feasibility of the thermodynamically controlled synthesis of crystalline sp3-carbon networks. We show that there is a critical pressure below which decomposition of the carbon network is favored and above which the carbon network is stable. Based on advanced, highly accurate quantum mechanical calculations using the all-electron full-potential linearized augmented plane-wave method (FP-LAPW) and the Birch–Murnaghan equation of state, this critical pressure is 26.5 GPa (viz. table of contents graphic). Such pressures are experimentally readily accessible and afford thermodynamic control for suppression of decomposition reactions. The present results further suggest that a general pattern of pressure-directed control exists for many isolobal conversions of sp2 to sp3 allotropes, relating not only to fluorocarbon chemistry but also extending to inorganic and solid-state materials science.

  7. Facile high-yield synthesis of polyaniline nanosticks with intrinsic stability and electrical conductivity.

    Science.gov (United States)

    Li, Xin-Gui; Li, Ang; Huang, Mei-Rong

    2008-01-01

    Chemical oxidative polymerization at 15 degrees C was used for the simple and productive synthesis of polyaniline (PAN) nanosticks. The effect of polymerization media on the yield, size, stability, and electrical conductivity of the PAN nanosticks was studied by changing the concentration and nature of the acid medium and oxidant and by introducing organic solvent. Molecular and supramolecular structure, size, and size distribution of the PAN nanosticks were characterized by UV/Vis and IR spectroscopy, X-ray diffraction, laser particle-size analysis, and transmission electron microscopy. Introduction of organic solvent is advantageous for enhancing the yield of PAN nanosticks but disadvantageous for formation of PAN nanosticks with small size and high conductivity. The concentration and nature of the acid medium have a major influence on the polymerization yield and conductivity of the nanosized PAN. The average diameter and length of PAN nanosticks produced with 2 M HNO(3) and 0.5 M H(2)SO(4) as acid media are about 40 and 300 nm, respectively. The PAN nanosticks obtained in an optimal medium (i.e., 2 M HNO(3)) exhibit the highest conductivity of 2.23 S cm(-1) and the highest yield of 80.7 %. A mechanism of formation of nanosticks instead of nanoparticles is proposed. Nanocomposite films of the PAN nanosticks with poly(vinyl alcohol) show a low percolation threshold of 0.2 wt %, at which the film retains almost the same transparency and strength as pure poly(vinyl alcohol) but 262 000 times the conductivity of pure poly(vinyl alcohol) film. The present synthesis of PAN nanosticks requires no external stabilizer and provides a facile and direct route for fabrication of PAN nanosticks with high yield, controllable size, intrinsic self-stability, strong redispersibility, high purity, and optimizable conductivity.

  8. Controlled synthesis and photocatalytic properties of rhombic dodecahedral Ag3PO4 with high surface energy

    International Nuclear Information System (INIS)

    Xie, Yao; Huang, Zhaohui; Zhang, Zhijie; Zhang, Xiaoguang; Wen, Ruilong; Liu, Yangai; Fang, Minghao; Wu, Xiaowen

    2016-01-01

    Graphical abstract: The high amount of rhombic dodecahedral Ag 3 PO 4 particles with a high exposure of the {110} facets and high surface energy (the surface energy of the {110} facets was 1.31 J/m 2 , greater than that of the {100} facet (1.12 J/m 2 ).) exhibited excellent photocatalytic activity. - Highlights: • High contents of rhombic dodecahedral Ag 3 PO 4 photocatalysts are prepared. • Excessive EG can destroy the morphology of Ag 3 PO 4 in synthesis process. • The rhombic dodecahedral Ag 3 PO 4 exhibits high surface energy. • High surface energy implies high photocatalytic activity. - Abstract: In this study, a series of Ag 3 PO 4 photocatalysts with different contents of rhombic dodecahedral particles were prepared in one pot by a facile, novel hydrothermal method using ethylene glycol (EG), which served as both a morphology modifier and reducing agent. The effects of EG content on the morphologies of Ag 3 PO 4 photocatalysts were discussed. The photocatalytic activity of the Ag 3 PO 4 photocatalysts was evaluated by the degradation of methylene blue trihydrate under visible-light irradiation. With the use of 0.8% EG in the reaction solvent, the sample exhibited excellent photocatalytic activity, attributed to the high amount of rhombic dodecahedral Ag 3 PO 4 particles with a high exposure of the {110} facets and high surface energy. The surface energy of the {110} facets was 1.31 J/m 2 , greater than that of the {100} facet (1.12 J/m 2 ). However, with 1% EG in the reaction solvent, although the Ag 3 PO 4 photocatalysts were composed of a majority of rhombic dodecahedral Ag 3 PO 4 particles, tiny Ag particles formed from Ag + under the action of EG attached on the surface of the sample decreased the absorption of visible light, resulting in low photocatalytic activity.

  9. Efficient Synthesis of Differentiated syn-1,2-Diol Derivatives by Asymmetric Transfer Hydrogenation-Dynamic Kinetic Resolution of α-Alkoxy-Substituted β-Ketoesters.

    Science.gov (United States)

    Monnereau, Laure; Cartigny, Damien; Scalone, Michelangelo; Ayad, Tahar; Ratovelomanana-Vidal, Virginie

    2015-08-10

    Asymmetric transfer hydrogenation was applied to a wide range of racemic aryl α-alkoxy-β-ketoesters in the presence of well-defined, commercially available, chiral catalyst Ru(II) -(N-p-toluenesulfonyl-1,2-diphenylethylenediamine) and a 5:2 mixture of formic acid and triethylamine as the hydrogen source. Under these conditions, dynamic kinetic resolution was efficiently promoted to provide the corresponding syn α-alkoxy-β-hydroxyesters derived from substituted aromatic and heteroaromatic aldehydes with a high level of diastereoselectivity (diastereomeric ratio (d.r.)>99:1) and an almost perfect enantioselectivity (enantiomeric excess (ee)>99 %). Additionally, after extensive screening of the reaction conditions, the use of Ru(II) - and Rh(III) -tethered precatalysts extended this process to more-challenging substrates that bore alkenyl-, alkynyl-, and alkyl substituents to provide the corresponding syn α-alkoxy-β-hydroxyesters with excellent enantiocontrol (up to 99 % ee) and good to perfect diastereocontrol (d.r.>99:1). Lastly, the synthetic utility of the present protocol was demonstrated by application to the asymmetric synthesis of chiral ester ethyl (2S)-2-ethoxy-3-(4-hydroxyphenyl)-propanoate, which is an important pharmacophore in a number of peroxisome proliferator-activated receptor α/γ dual agonist advanced drug candidates used for the treatment of type-II diabetes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Application of Self-Propagating High Temperature Synthesis to the Fabrication of Actinide Bearing Nitride and Other Ceramic Nuclear Fuels

    International Nuclear Information System (INIS)

    Moore, John J.; Reigel, Marissa M.; Donohoue, Collin D.

    2009-01-01

    The project uses an exothermic combustion synthesis reaction, termed self-propagating high-temperature synthesis (SHS), to produce high quality, reproducible nitride fuels and other ceramic type nuclear fuels (cercers and cermets, etc.) in conjunction with the fabrication of transmutation fuels. The major research objective of the project is determining the fundamental SHS processing parameters by first using manganese as a surrogate for americium to produce dense Zr-Mn-N ceramic compounds. These fundamental principles will then be transferred to the production of dense Zr-Am-N ceramic materials. A further research objective in the research program is generating fundamental SHS processing data to the synthesis of (i) Pu-Am-Zr-N and (ii) U-Pu-Am-N ceramic fuels. In this case, Ce will be used as the surrogate for Pu, Mn as the surrogate for Am, and depleted uranium as the surrogate for U. Once sufficient fundamental data has been determined for these surrogate systems, the information will be transferred to Idaho National Laboratory (INL) for synthesis of Zr-Am-N, Pu-Am-Zr-N and U-Pu-Am-N ceramic fuels. The high vapor pressures of americium (Am) and americium nitride (AmN) are cause for concern in producing nitride ceramic nuclear fuel that contains Am. Along with the problem of Am retention during the sintering phases of current processing methods, are additional concerns of producing a consistent product of desirable homogeneity, density and porosity. Similar difficulties have been experienced during the laboratory scale process development stage of producing metal alloys containing Am wherein compact powder sintering methods had to be abandoned. Therefore, there is an urgent need to develop a low-temperature or low-heat fuel fabrication process for the synthesis of Am-containing ceramic fuels. Self-propagating high temperature synthesis (SHS), also called combustion synthesis, offers such an alternative process for the synthesis of Am nitride fuels. Although SHS

  11. Impact of high altitude on the hepatic fatty acid oxidation and synthesis in rats

    Energy Technology Data Exchange (ETDEWEB)

    Ni, Qian [Department of General Surgery, Hepatic-biliary-pancreatic Institute, Lanzhou University Second Hospital, Lanzhou (China); Department of Pediatrics, Lanzhou University Second Hospital, Lanzhou (China); Shao, Yuan; Wang, Ying Zhen [Department of General Surgery, Hepatic-biliary-pancreatic Institute, Lanzhou University Second Hospital, Lanzhou (China); Jing, Yu Hong [Institute of Anatomy, School of Basic Medicine, Lanzhou University, Lanzhou (China); Zhang, You Cheng, E-mail: zhangychmd@126.com [Department of General Surgery, Hepatic-biliary-pancreatic Institute, Lanzhou University Second Hospital, Lanzhou (China)

    2014-04-04

    Highlights: • Acute exposure to high altitude (HA) increased hepatic fatty acid (FA) β-oxidation. • Acute exposure of rats to HA increased hepatic FA synthesis. • PPARα and AMPK can regulate the FA metabolism. • FA may be a key energy fuel and a compensation for CHO during acute exposure to HA. • The acute changes of FA metabolism may be a mechanism of acclimatization. - Abstract: High altitude (HA) affects energy metabolism. The impact of acute and chronic HA acclimatization on the major metabolic pathways is still controversial. In this study, we aimed to unveil the impact of HA on the key enzymes involved in the fatty acid (FA) metabolism in liver. Rats were exposed to an altitude of 4300 m for 30 days and the expressions of two key proteins involved in FA β-oxidation (carnitine palmitoyl transferase I, CPT-I; and peroxisome proliferator-activated receptor alpha, PPARα), two proteins involved in FA synthesis (acetyl CoA carboxylase-1, ACC-1; and AMP-activated protein kinase, AMPK), as well as the total ketone body in the liver and the plasma FFAs were examined. Rats without HA exposure were used as controls. We observed that the acute exposure of rats to HA (3 days) led to a significant increase in the expressions of CPT-I and PPARα and in the total hepatic ketone body. Longer exposure (15 days) caused a marked decrease in the expression of CPT-I and PPARα. By 30 days after HA exposure, the expression levels of CPT-I and PPARα returned to the control level. The hepatic ACC-1 level showed a significant increase in rats exposed to HA for 1 and 3 days. In contrast, the hepatic level of AMPK showed a significant reduction throughout the experimental period. Plasma FFA concentrations did not show any significant changes following HA exposure. Thus, increased hepatic FA oxidation and synthesis in the early phase of HA exposure may be among the important mechanisms for the rats to respond to the hypoxic stress in order to acclimatize themselves to the

  12. Impact of high altitude on the hepatic fatty acid oxidation and synthesis in rats

    International Nuclear Information System (INIS)

    Ni, Qian; Shao, Yuan; Wang, Ying Zhen; Jing, Yu Hong; Zhang, You Cheng

    2014-01-01

    Highlights: • Acute exposure to high altitude (HA) increased hepatic fatty acid (FA) β-oxidation. • Acute exposure of rats to HA increased hepatic FA synthesis. • PPARα and AMPK can regulate the FA metabolism. • FA may be a key energy fuel and a compensation for CHO during acute exposure to HA. • The acute changes of FA metabolism may be a mechanism of acclimatization. - Abstract: High altitude (HA) affects energy metabolism. The impact of acute and chronic HA acclimatization on the major metabolic pathways is still controversial. In this study, we aimed to unveil the impact of HA on the key enzymes involved in the fatty acid (FA) metabolism in liver. Rats were exposed to an altitude of 4300 m for 30 days and the expressions of two key proteins involved in FA β-oxidation (carnitine palmitoyl transferase I, CPT-I; and peroxisome proliferator-activated receptor alpha, PPARα), two proteins involved in FA synthesis (acetyl CoA carboxylase-1, ACC-1; and AMP-activated protein kinase, AMPK), as well as the total ketone body in the liver and the plasma FFAs were examined. Rats without HA exposure were used as controls. We observed that the acute exposure of rats to HA (3 days) led to a significant increase in the expressions of CPT-I and PPARα and in the total hepatic ketone body. Longer exposure (15 days) caused a marked decrease in the expression of CPT-I and PPARα. By 30 days after HA exposure, the expression levels of CPT-I and PPARα returned to the control level. The hepatic ACC-1 level showed a significant increase in rats exposed to HA for 1 and 3 days. In contrast, the hepatic level of AMPK showed a significant reduction throughout the experimental period. Plasma FFA concentrations did not show any significant changes following HA exposure. Thus, increased hepatic FA oxidation and synthesis in the early phase of HA exposure may be among the important mechanisms for the rats to respond to the hypoxic stress in order to acclimatize themselves to the

  13. Synthesis of nanoparticles using high-pressure sputtering for magnetic domain imaging

    International Nuclear Information System (INIS)

    Shah, Prasanna; Gavrin, A.

    2006-01-01

    We have developed a modified sputtering gun for direct synthesis of metallic nanoparticles, and used this system to produce magnetic domain images using high-resolution Bitter microscopy (HRBM). The nanoparticles are produced at 900 mTorr inside the gun and transported to the main vacuum chamber by the pressure difference between the chamber and the gun interior. Fe particles synthesized using the particle gun have been characterized using X-ray diffraction, atomic force microscopy, and transmission electron microscopy techniques. The particles are 15-30 nm in size with a pure BCC phase. Further, we have deposited these Fe nanoparticles on magnetic recording media and observed the domain patterns using optical microscopy, scanning electron microscopy, and atomic force microscopy. We achieve a spatial resolution of at most 80 nm

  14. Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

    Science.gov (United States)

    Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

    2013-11-01

    A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl11O18 and Ce2SiO5. The leaching rate of cerium over a period of 28 days was 10-5-10-6 g/(m2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products.

  15. Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

    International Nuclear Information System (INIS)

    Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

    2013-01-01

    A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl 11 O 18 and Ce 2 SiO 5 . The leaching rate of cerium over a period of 28 days was 10 −5 –10 −6 g/(m 2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products

  16. Synthesis of gold nanoflowers using deep eutectic solvent with high surface enhanced Raman scattering properties

    Science.gov (United States)

    Aghakhani Mahyari, Farzaneh; Tohidi, Maryam; Safavi, Afsaneh

    2016-09-01

    A facile, seed-less and one-pot method was developed for synthesis of gold nanoflowers with multiple tips through reduction of HAuCl4 with deep eutectic solvent at room temperature. This solvent is eco-friendly, low-cost, non-toxic and biodegradable and can act as both reducing and shape-controlling agent. In this protocol, highly branched and stable gold nanoflowers were obtained without using any capping agent. The obtained products were characterized by different techniques including, field emission scanning electron microscopy, transmission electron microscopy, x-ray diffraction and UV-vis spectroscopy. The as-prepared gold nanoflowers exhibit efficient surface-enhanced Raman scattering (SERS) properties which can be used as excellent substrates for SERS.

  17. Synthesis and high temperature stability of amorphous Si(B)CN-MWCNT composite nanowires

    Science.gov (United States)

    Bhandavat, Romil; Singh, Gurpreet

    2012-02-01

    We demonstrate synthesis of a hybrid nanowire structure consisting of an amorphous polymer-derived silicon boron-carbonitride (Si-B-C-N) shell with a multiwalled carbon nanotube core. This was achieved through a novel process involving preparation of a boron-modified liquid polymeric precursor through a reaction of trimethyl borate and polyureasilazane under atmospheric conditions; followed by conversion of polymer to glass-ceramic on carbon nanotube surfaces through controlled heating. Chemical structure of the polymer was studied by liquid-NMR while evolution of various ceramic phases was studied by Raman spectroscopy, solid-NMR, Fourier transform infrared and X-ray photoelectron spectroscopy. Electron microscopy and X-ray diffraction confirms presence of amorphous Si(B)CN coating on individual nanotubes for all specimen processed below 1400 degree C. Thermogravimetric analysis, followed by TEM revealed high temperature stability of the carbon nanotube core in flowing air up to 1300 degree C.

  18. A Novel and Highly Regioselective Synthesis of New Carbamoylcarboxylic Acids from Dianhydrides

    Directory of Open Access Journals (Sweden)

    Adrián Ochoa-Terán

    2014-01-01

    Full Text Available A regioselective synthesis has been developed for the preparation of a series of N,N′-disubstituted 4,4′-carbonylbis(carbamoylbenzoic acids and N,N′-disubstituted bis(carbamoyl terephthalic acids by treatment of 3,3′,4,4′-benzophenonetetracarboxylic dianhydride (1 and 1,2,4,5-benzenetetracarboxylic dianhydride (2 with arylalkyl primary amines (A-N. The carbamoylcarboxylic acid derivatives were synthesized with good yield and high purity. The specific reaction conditions were established to obtain carbamoyl and carboxylic acid functionalities over the thermodynamically most favored imide group. Products derived from both anhydrides 1 and 2 were isolated as pure regioisomeric compounds under innovative experimental conditions. The chemo- and regioselectivity of products derived from dianhydrides were determined by NMR spectroscopy and confirmed by density functional theory (DFT. All products were characterized by NMR, FTIR, and MS.

  19. Facile and High-Yielding Synthesis of TAM Biradicals and Monofunctional TAM Radicals.

    Science.gov (United States)

    Trukhin, Dmitry V; Rogozhnikova, Olga Yu; Troitskaya, Tatiana I; Vasiliev, Vladimir G; Bowman, Michael K; Tormyshev, Victor M

    2016-04-01

    Facile and high-yielding procedures for synthesis of monocarboxylic acid derivatives of triarylmethyl radicals (TAMs) were developed. Reaction of methyl thioglycolate with tris(2,3,5,6-tetrathiaaryl)methyl cation smoothly afforded the monosubstituted TAM derivative, which was hydrolyzed to a monocarboxylic acid, with the TAM moiety attached to thioglycolic acid via the sulfur atom. Alternatively, the diamagnetic tricarboxylic acid precursor of Finland trityl was transformed to a trimethyl ester and partially hydrolyzed under controlled conditions. The diester product was isolated and the remaining fractions were converted back to the trimethyl ester for production of more diester. The first representatives of TAM biradicals with different TAM cores and interspin distances were obtained by reaction of these new TAM monocaboxylic acids with N,N'-dimethylethylenediamine.

  20. Self-propagating high-temperature synthesis of TiC-WC composite materials

    International Nuclear Information System (INIS)

    Mas-Guindal, M.J.; Contreras, L.; Turrillas, X.; Vaughan, G.B.M.; Kvick, A.; Rodriguez, M.A.

    2006-01-01

    TiC-WC composites have been obtained in situ by self-propagating high-temperature synthesis (SHS) from a mixture of compacted powders of elemental titanium, tungsten and graphite. The Rietveld method has proved to be a useful tool to quantify the different phases in the reaction and calculate the cell parameters of the solid solution found in the products. The reaction has also been followed in real time by X-ray diffraction at the European Synchrotron Radiation Facility (ESRF ID-11 Materials Science Beamline). The mechanism of the reaction is discussed in terms of the diffusion of liquid titanium to yield titanium carbide with a solid solution of tungsten. The microstructures of the materials obtained by this method are presented

  1. Phase 1 Final Technical Report - MgB2 Synthesis: Pushing to High Field Performance

    International Nuclear Information System (INIS)

    Bhatia, Mohit; McIntyre, Peter

    2009-01-01

    crystalline boron results in the formation of parasitic phases such as MgB4, MgB7, etc. Such parasitic phases are a primary element of the connectivity problem, in which even though a sample powder may contain grains of high-quality MgB2, adjacent grains are surrounded by intergrowths of parasitic phases so that current trans-port is badly degraded. The best results to date have been obtained using boron powder produced long ago for a rocket propellant development project. The synthesis process was complex and is now largely lost, and the manufacturing equipment has long since been scrapped. The last batch of the powder has been used during recent years to support MgB2 R and D at several labs, but supplies are dwindling. ATC has identified a first application of its plasma torch to synthesize phase-pure amorphous boron flake using a rapid-quench splat technique. Inexpensive technical-grade boron would be purified of contaminants, then dispersed as an aerosol in inert gas and passed through the plasma torch to melt it into a spray. The spray would be splat-condensed on a rotating drum to form pure amorphous flake. The process would begin with technical-grade boron powder, having good stoichiometric purity, nanoscale particles, but significant contamination of MgO and crystalline boron. We used wet chemistry to remove B2O3 completely and reduced the MgO impurity, and analyzed the particle size distribution using a Coulter counter and the phase composition using X-ray diffrac-tion (XRD). The next step will be to build an rf plasma torch with a recirculating single-component aerosol feed and the cooled splat drum and collector, and undertake process devel-opment for amorphous boron powder. This revised goal has two benefits. First, it is an easier technology than our ultimate goal of a multi-component laminar flow torch. We have been counseled by those experienced in plasma torch technology that our ultimate goal will require a torch that should be feasible but has never been

  2. Nacre-Templated Synthesis of Highly Dispersible Carbon Nanomeshes for Layered Membranes with High-Flux Filtration and Sensing Properties.

    Science.gov (United States)

    Kong, Meng; Li, Mingjie; Shang, Ruoxu; Wu, Jingyu; Yan, Peisong; Xu, Dongmei; Li, Chaoxu

    2018-01-24

    Marine shells not only represent a rapidly accumulating type of fishery wastes but also offer a unique sort of hybrid nanomaterials produced greenly and massively in nature. The elaborate "brick and mortar" structures of nacre enabled the synthesis of carbon nanomeshes with <1 nm thickness, hierarchical porosity, and high specific surface area through pyrolysis, in which two-dimensional (2D) organic layers served as the carbonaceous precursor and aragonite platelets as the hard template. Mineral bridges within 2D organic layers templated the formation of mesh pores of 20-70 nm. In contrast to other hydrophobic carbon nanomaterials, these carbon nanomeshes showed super dispersibility in diverse solvents and thus processability for membranes through filtration, patterning, spray-coating, and ink-writing. The carbon membranes with layered structures were capable of serving not only for high-flux filtration and continuous flow absorption but also for electrochemical and strain sensing with high sensitivity. Thus, utilization of marine shells, on one hand, relieves the environmental concern of shellfish waste, on the other hand, offers a facile, green, low-cost, and massive approach to synthesize unique carbon nanomeshes alternative to graphene nanomeshes and applicable in environmental adsorption, filtration, wearable sensors, and flexible microelectronics.

  3. Synthesis of uniform CdS nanowires in high yield and its single nanowire electrical property

    International Nuclear Information System (INIS)

    Yan Shancheng; Sun Litao; Qu Peng; Huang Ninping; Song Yinchen; Xiao Zhongdang

    2009-01-01

    Large-scale high quality CdS nanowires with uniform diameter were synthesized by using a rapid and simple solvothermal route. Field emission scan electron microscopy (FESEM) and transmission electron microscopy (TEM) images show that the CdS nanowires have diameter of about 26 nm and length up to several micrometres. High resolution TEM (HRTEM) study indicates the single-crystalline nature of CdS nanowires with an oriented growth along the c-axis direction. The optical properties of the products were characterized by UV-vis absorption spectra, photoluminescence spectra and Raman spectra. The resistivity, electron concentration and electron mobility of single NW are calculated by fitting the symmetric I-V curves measured on single NW by the metal-semiconductor-metal model based on thermionic field emission theory. - Graphical abstract: Large-scale high quality CdS nanowires (NWs) with uniform diameter were synthesized by using a rapid and simple solvothermal route. The reaction time is reduced to 2 h, comparing to other synthesis which needed long reaction time up to 12 h. In addition, the as-prepared CdS nanowires have more uniform diameter and high yield. More importantly, the I-V curve of present single CdS nanowire has a good symmetric characteristic as expected by the theory.

  4. Method of synthesis of abstract images with high self-similarity

    Science.gov (United States)

    Matveev, Nikolay V.; Shcheglov, Sergey A.; Romanova, Galina E.; Koneva, Ð.¢atiana A.

    2017-06-01

    Abstract images with high self-similarity could be used for drug-free stress therapy. This based on the fact that a complex visual environment has a high affective appraisal. To create such an image we can use the setup based on the three laser sources of small power and different colors (Red, Green, Blue), the image is the pattern resulting from the reflecting and refracting by the complicated form object placed into the laser ray paths. The images were obtained experimentally which showed the good therapy effect. However, to find and to choose the object which gives needed image structure is very difficult and requires many trials. The goal of the work is to develop a method and a procedure of finding the object form which if placed into the ray paths can provide the necessary structure of the image In fact the task means obtaining the necessary irradiance distribution on the given surface. Traditionally such problems are solved using the non-imaging optics methods. In the given case this task is very complicated because of the complicated structure of the illuminance distribution and its high non-linearity. Alternative way is to use the projected image of a mask with a given structure. We consider both ways and discuss how they can help to speed up the synthesis procedure for the given abstract image of the high self-similarity for the setups of drug-free therapy.

  5. Carbamoyl anion-initiated cascade reaction for stereoselective synthesis of substituted α-hydroxy-β-amino amides.

    Science.gov (United States)

    Lin, Chao-Yang; Ma, Peng-Ju; Sun, Zhao; Lu, Chong-Dao; Xu, Yan-Jun

    2016-01-18

    A carbamoyl anion-initiated cascade reaction with acylsilanes and imines has been used to rapidly construct substituted α-hydroxy-β-amino amides. The Brook rearrangement-mediated cascade allows the formation of two C-C bonds and one O-Si bond in a single pot. Using this approach, a range of α-aryl α-hydroxy-β-amino amides has been synthesized in high yields with excellent diastereoselectivities.

  6. Synthesis and chemical recycling of high polymers using C1 compounds; C1 kagobutsu ni yoru kobunshi no chemical recycle

    Energy Technology Data Exchange (ETDEWEB)

    Masuda, T. [National Institute of Materials and Chemical Research, Tsukuba (Japan)

    1997-09-01

    The paper outlined a study of the synthesis of high polymers using C1 compounds which are continuously usable chemical materials and the related compounds such as the derivatives, and also the chemical recycle. In the case of waste plastics mixed in urban refuse, effective is the chemical recycle where C1 compounds obtained by gasifying the mixed waste are used as high polymer material. For the synthesis and recycle of high polymers using C1 compounds, there are three routes: Route A (recycle via high polymer materials), Route B (recycle via C1 compounds and high polymer materials), and Route C including global-scale carbon recycle (recycle via carbon dioxide from biodegradable plastics using microorganism). Among high polymers, those that can be synthesized from C1 compounds, for example, polymethylene, polyacetal and polyketone can be chemically recycled by Route B. 30 refs., 2 figs., 1 tab.

  7. Controllable synthesis of nickel bicarbonate nanocrystals with high homogeneity for a high-performance supercapacitor

    Science.gov (United States)

    Gu, Jianmin; Liu, Xin; Wang, Zhuang; Bian, Zhenpan; Jin, Cuihong; Sun, Xiao; Yin, Baipeng; Wu, Tianhui; Wang, Lin; Tang, Shoufeng; Wang, Hongchao; Gao, Faming

    2017-08-01

    The electrochemical performance of supercapacitors might be associated with the homogeneous structure of the electrode materials. However, the relationship between the degree of uniformity for the electrode materials and the electrochemical performance of the supercapacitor is not clear. Herein, we synthesize two types of nickel bicarbonate nanocrystals with different degrees of uniformity to investigate this relationship. As the electroactive material, the nickel bicarbonate nanocrystals with a homogeneous structure could provide a larger space and offer more exposed atoms for the electrochemical reaction than the nanocrystals with a heterogeneous structure. The homogeneous nickel bicarbonate nanocrystals exhibit better electrochemical performance and show excellent specific capacitance (1596 F g-1 at 2 A g-1 and 1260 F g-1 at 30 A g-1), which is approximately twice that of the heterogeneous nickel bicarbonate nanocrystals. The cycling stability for the homogeneity (˜80%) is higher than the inhomogeneity (˜61%) at a high current density of 5 A g-1.

  8. Bacillus megaterium sporal peptidoglycan synthesis studied by high-resolution autoradiography.

    Science.gov (United States)

    Frehel, C; Ryter, A

    1980-11-01

    Cells of a Dap- Lys- mutant strain of Bacillus megaterium were pulse labeled with [3H]diaminopimelic acid at different times of growth and sporulation. They were processed for radioactivity measurements and high-resolution autoradiography either just after the pulse or after a chase in a nonradioactive medium until refractile forespores started to appear at time (t)4,5. In the pulse-labeled cells, autoradiographs and radioactivity measurements showed that the radioactivity incorporated during a pulse decreased abruptly after t0 and stayed at a low level until t5, although the forespore wall and cortex were formed between t4 and t5. In the pulse-chased bacteria, the acid-insoluble radioactivity, as well as the number of silver grains on autoradiographs, increased during the chase in cells labeled at t1 to t2, whereas it decreased in those labeled before t0. Furthermore, analysis of silver grain distribution showed that, in stage IV bacteria, grains were distributed at the outside of the forespore, mostly on the sporangium cell wall, when pulse-labeling occurred before or at t0; they were located along the cortex and in the forespore cytoplasm when labeling was made at t1 or t2. These facts show that [3H]diaminopimelic acid necessary for spore envelope synthesis was incorporated before their morphological appearance. Free or small diaminopimelic acid precursors entered the sporangium between t1 and t2. The appearance of silver grains in the forespore cytoplasm suggests that the forespore is implicated in sporal peptidoglycan synthesis.

  9. Phase controlled synthesis of (Mg, Ca, Ba)-ferrite magnetic nanoparticles with high uniformity

    International Nuclear Information System (INIS)

    Wang, S.F.; Li, Q.; Zu, X.T.; Xiang, X.; Liu, W.; Li, S.

    2016-01-01

    (Mg, Ca, Ba)-ferrite magnetic nanoparticles were successfully synthesized through modifying the atomic ratio of polysaccharide and chelating agent at an optimal sintering temperature. In the process, the polysaccharide plays an important role in drastically shrinking the precursor during the gel drying process. In the metal-complex structure, M"2"+ ion active sites were coordinated by −OH of the water molecules except for EDTA anions. The MFe_2O_4 magnetic nanoparticles exhibited enhanced magnetic properties when compared with nano-MFe_2O_4 of similar particle size synthesized by other synthesis route reported in the literature. In particular, the sintering temperature improves the crystallinity and increases the hysteresis loop squareness ratio of (Mg, Ca, Ba)-ferrite nanoparticles significantly. - Graphical abstract: Schematic representation of the proposed model for MFe_2O_4 nanoparticle synthesis, starting from EDTA-chelated M"2"+ (M=Mg, Ca, or Ba) cations (left). High dispersion (Mg, Ca, Ba)-ferrite magnetic nanoparticles were prepared by a modified polyacrylamide gel route. Optimized utilization of polysaccharide, chelating agent, and sintering temperature allowed the formation of (Mg, Ca, Ba)-ferrite nanoparticles with a narrow diameter distribution. - Highlights: • We report a modified polyacrylamide gel route to synthesize (Mg, Ca, Ba)-ferrite magnetic nanoparticles. • Chelate mechanism of metal ions (Mg, Ca, Ba) and EDTA has been discussed. • Phase transformation process of (Mg, Ca, Ba)-ferrites has been discussed. • The preparation method increases the hysteresis loop squareness ratio of (Mg, Ca, Ba)-ferrite nanoparticles.

  10. Phase controlled synthesis of (Mg, Ca, Ba)-ferrite magnetic nanoparticles with high uniformity

    Energy Technology Data Exchange (ETDEWEB)

    Wang, S.F., E-mail: wangshifa2006@yeah.net [School of Physical Electronics, University of Electronic Science and Technology of China, Chengdu 610054, Sichuan (China); Science and technology on vacuum technology and physics laboratory, Lanzhou Institute of Physics, Lanzhou 730000, Gansu (China); Li, Q. [School of Physical Electronics, University of Electronic Science and Technology of China, Chengdu 610054, Sichuan (China); Zu, X.T., E-mail: xtzu@uestc.edu.cn [Institute of Fundamental and Frontier Sciences, University of Electronic Science and Technology of China, Chengdu 610054, Sichuan (China); Xiang, X.; Liu, W. [School of Physical Electronics, University of Electronic Science and Technology of China, Chengdu 610054, Sichuan (China); Li, S., E-mail: sean.li@unsw.edu.au [School of Material Science and Engineering, University of New South Wales, Sydney 2052 (Australia)

    2016-12-01

    (Mg, Ca, Ba)-ferrite magnetic nanoparticles were successfully synthesized through modifying the atomic ratio of polysaccharide and chelating agent at an optimal sintering temperature. In the process, the polysaccharide plays an important role in drastically shrinking the precursor during the gel drying process. In the metal-complex structure, M{sup 2+} ion active sites were coordinated by −OH of the water molecules except for EDTA anions. The MFe{sub 2}O{sub 4} magnetic nanoparticles exhibited enhanced magnetic properties when compared with nano-MFe{sub 2}O{sub 4} of similar particle size synthesized by other synthesis route reported in the literature. In particular, the sintering temperature improves the crystallinity and increases the hysteresis loop squareness ratio of (Mg, Ca, Ba)-ferrite nanoparticles significantly. - Graphical abstract: Schematic representation of the proposed model for MFe{sub 2}O{sub 4} nanoparticle synthesis, starting from EDTA-chelated M{sup 2+} (M=Mg, Ca, or Ba) cations (left). High dispersion (Mg, Ca, Ba)-ferrite magnetic nanoparticles were prepared by a modified polyacrylamide gel route. Optimized utilization of polysaccharide, chelating agent, and sintering temperature allowed the formation of (Mg, Ca, Ba)-ferrite nanoparticles with a narrow diameter distribution. - Highlights: • We report a modified polyacrylamide gel route to synthesize (Mg, Ca, Ba)-ferrite magnetic nanoparticles. • Chelate mechanism of metal ions (Mg, Ca, Ba) and EDTA has been discussed. • Phase transformation process of (Mg, Ca, Ba)-ferrites has been discussed. • The preparation method increases the hysteresis loop squareness ratio of (Mg, Ca, Ba)-ferrite nanoparticles.

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

    Science.gov (United States)

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

  12. Hydrothermal synthesis of high surface area ZIF-8 with minimal use of TEA

    Science.gov (United States)

    Butova, V. V.; Budnyk, A. P.; Bulanova, E. A.; Lamberti, C.; Soldatov, A. V.

    2017-07-01

    In this paper we present, for the first time, a simple hydrothermal recipe for the synthesis of ZIF-8 Metal-Organic Framework (MOF) with a large specific surface area (1340 m2/g by BET). An important feature of the method is that the product forms in aqueous medium under standard hydrothermal conditions without DMF and great excess of linker with the use of TEA as structure directing agent. The ZIF-8 crystal phase of the product was confirmed by XRD; this technique has been also exploited to check the crystallinity and to follow the changes in the MOF structure induced by heating. TGA and temperature dependent XRD testify the high thermal stability of the material (470 °C in N2 and at 400 °C in air). The IR spectral profile of the material provides a complete picture of vibrations assigned to the linker and the metal center. The systematic investigation of the products obtained by increasing the TEA amount in the reacting medium from 0 to 25.5 mol equivalent Zn2+, allowed us to understand its role and to find 2.6 mol equivalent Zn2+ as the minimum amount needed to obtain a single phase ZIF-8 material with the high standard reported above. The stability of the material under severe basic conditions makes it a promising candidate in heterogeneous catalysis. The material has shown high capacity in I2 uptake, making it interesting also for selective molecular adsorption.

  13. A hardware acceleration based on high-level synthesis approach for glucose-insulin analysis

    Science.gov (United States)

    Daud, Nur Atikah Mohd; Mahmud, Farhanahani; Jabbar, Muhamad Hairol

    2017-01-01

    In this paper, the research is focusing on Type 1 Diabetes Mellitus (T1DM). Since this disease requires a full attention on the blood glucose concentration with the help of insulin injection, it is important to have a tool that able to predict that level when consume a certain amount of carbohydrate during meal time. Therefore, to make it realizable, a Hovorka model which is aiming towards T1DM is chosen in this research. A high-level language is chosen that is C++ to construct the mathematical model of the Hovorka model. Later, this constructed code is converted into intellectual property (IP) which is also known as a hardware accelerator by using of high-level synthesis (HLS) approach which able to improve in terms of design and performance for glucose-insulin analysis tool later as will be explained further in this paper. This is the first step in this research before implementing the design into system-on-chip (SoC) to achieve a high-performance system for the glucose-insulin analysis tool.

  14. Methylcellulose-Directed Synthesis of Nanocrystalline Zeolite NaA with High CO₂ Uptake.

    Science.gov (United States)

    Shakarova, Dilshod; Ojuva, Arto; Bergström, Lennart; Akhtar, Farid

    2014-07-28

    Zeolite NaA nanocrystals with a narrow particle size distribution were prepared by template-free hydrothermal synthesis in thermo-reversible methylcellulose gels. The effects of the amount of methylcellulose, crystallization time and hydrothermal treatment temperature on the crystallinity and particle size distribution of the zeolite NaA nanocrystals were investigated. We found that the thermogelation of methylcellulose in the alkaline Na₂O-SiO₂-Al₂O₃-H₂O system played an important role in controlling the particle size. The synthesized zeolite nanocrystals are highly crystalline, as demonstrated by X-ray diffraction (XRD), and scanning electron microscopy (SEM) shows that the nanocrystals can also display a well-defined facetted morphology. Gas adsorption studies on the synthesized nanocrystalline zeolite NaA showed that nanocrystals with a size of 100 nm displayed a high CO₂ uptake capacity (4.9 mmol/g at 293 K at 100 kPa) and a relatively rapid uptake rate compared to commercially available, micron-sized particles. Low-cost nanosized zeolite adsorbents with a high and rapid uptake are important for large scale gas separation processes, e.g., carbon capture from flue gas.

  15. High-purity Cu nanocrystal synthesis by a dynamic decomposition method

    Science.gov (United States)

    Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

    2014-12-01

    Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

  16. Review of electric discharge microplasmas generated in highly fluctuating fluids: Characteristics and application to nanomaterials synthesis

    International Nuclear Information System (INIS)

    Stauss, Sven; Terashima, Kazuo; Muneoka, Hitoshi; Urabe, Keiichiro

    2015-01-01

    Plasma-based fabrication of novel nanomaterials and nanostructures is indispensible for the development of next-generation electronic devices and for green energy applications. In particular, controlling the interactions between plasmas and materials interfaces, and the plasma fluctuations, is crucial for further development of plasma-based processes and bottom-up growth of nanomaterials. Electric discharge microplasmas generated in supercritical fluids represent a special class of high-pressure plasmas, where fluctuations on the molecular scale influence the discharge properties and the possible bottom-up growth of nanomaterials. This review discusses an anomaly observed for direct current microplasmas generated near the critical point, a local decrease in the breakdown voltage. This anomalous behavior is suggested to be caused by the concomitant decrease of the ionization potential due to the formation of clusters near the critical point, and the formation of extended electron mean free paths caused by the high-density fluctuation near the critical point. It is also shown that in the case of dielectric barrier microdischarges generated close to the critical point, the high-density fluctuation of the supercritical fluid persists. The final part of the review discusses the application of discharges generated in supercritical fluids to synthesis of nanomaterials, in particular, molecular diamond—so-called diamondoids—by microplasmas generated inside conventional batch-type and continuous flow microreactors

  17. Facile Synthesis Polyethylene Glycol Coated Magnetite Nanoparticles for High Colloidal Stability

    Directory of Open Access Journals (Sweden)

    Mun Foong Tai

    2016-01-01

    Full Text Available Polyethylene glycol (PEG is one of the most frequently used synthetic polymers for surface modifications of magnetite nanoparticles (MNPs to provide a new opportunity for constructing high colloidal stability. Herein, a facile in situ coprecipitation technique is described for the synthesis of PEG coated MNPs using ammonium hydroxide as the precipitating agent. The structure and morphology of the prepared PEG coated MNPs samples were characterized by Fourier transform infrared (FTIR spectroscopy, X-ray spectroscopy, thermogravimetric analysis (TGA, and the high resolution transmission electron microscopy (HRTEM. In this study, all samples demonstrated hydrodynamic size in the range of 32 to 43 nm with narrow size distribution. In addition, the magnetic properties of resultant samples were investigated using a vibrating sample magnetometer (VSM to reveal the superparamagnetic behaviour with saturation magnetization. The saturation magnetization of PEG coated MNPs samples was in the range of 63 to 66 emu/g at 300 K. Interestingly, it was found that 1.0 g of PEG coated MNPs exhibited high colloidal stability in a basic solution (pH = 10 and nitrile (NBR latex up to 21 days as compared to the unmodified MNPs during the sedimentation test.

  18. Habituation to low or high protein intake does not modulate basal or postprandial muscle protein synthesis rates: a randomized trial.

    Science.gov (United States)

    Gorissen, Stefan Hm; Horstman, Astrid Mh; Franssen, Rinske; Kouw, Imre Wk; Wall, Benjamin T; Burd, Nicholas A; de Groot, Lisette Cpgm; van Loon, Luc Jc

    2017-02-01

    Muscle mass maintenance is largely regulated by basal muscle protein synthesis rates and the ability to increase muscle protein synthesis after protein ingestion. To our knowledge, no previous studies have evaluated the impact of habituation to either low protein intake (LOW PRO) or high protein intake (HIGH PRO) on the postprandial muscle protein synthetic response. We assessed the impact of LOW PRO compared with HIGH PRO on basal and postprandial muscle protein synthesis rates after the ingestion of 25 g whey protein. Twenty-four healthy, older men [age: 62 ± 1 y; body mass index (in kg/m 2 ): 25.9 ± 0.4 (mean ± SEM)] participated in a parallel-group randomized trial in which they adapted to either a LOW PRO diet (0.7 g · kg -1 · d -1 ; n = 12) or a HIGH PRO diet (1.5 g · kg -1 · d -1 ; n = 12) for 14 d. On day 15, participants received primed continuous l-[ring- 2 H 5 ]-phenylalanine and l-[1- 13 C]-leucine infusions and ingested 25 g intrinsically l-[1- 13 C]-phenylalanine- and l-[1- 13 C]-leucine-labeled whey protein. Muscle biopsies and blood samples were collected to assess muscle protein synthesis rates as well as dietary protein digestion and absorption kinetics. Plasma leucine concentrations and exogenous phenylalanine appearance rates increased after protein ingestion (P 0.05). Plasma exogenous phenylalanine availability over the 5-h postprandial period was greater after LOW PRO than after HIGH PRO (61% ± 1% compared with 56% ± 2%, respectively; P protein synthesis rates increased from 0.031% ± 0.004% compared with 0.039% ± 0.007%/h in the fasted state to 0.062% ± 0.005% compared with 0.057% ± 0.005%/h in the postprandial state after LOW PRO compared with HIGH PRO, respectively (P protein-derived amino acids in the circulation and does not lower basal muscle protein synthesis rates or increase postprandial muscle protein synthesis rates after ingestion of 25 g protein in older men. This trial was registered at clinicaltrials.gov as NCT

  19. One-Step Synthesis of Microporous Carbon Monoliths Derived from Biomass with High Nitrogen Doping Content for Highly Selective CO2 Capture

    OpenAIRE

    Geng, Zhen; Xiao, Qiangfeng; Lv, Hong; Li, Bing; Wu, Haobin; Lu, Yunfeng; Zhang, Cunman

    2016-01-01

    The one-step synthesis method of nitrogen doped microporous carbon monoliths derived from biomass with high-efficiency is developed using a novel ammonia (NH3)-assisted activation process, where NH3 serves as both activating agent and nitrogen source. Both pore forming and nitrogen doping simultaneously proceed during the process, obviously superior to conventional chemical activation. The as-prepared nitrogen-doped active carbons exhibit rich micropores with high surface area and high nitrog...

  20. High-throughput continuous hydrothermal synthesis of an entire nanoceramic phase diagram.

    Science.gov (United States)

    Weng, Xiaole; Cockcroft, Jeremy K; Hyett, Geoffrey; Vickers, Martin; Boldrin, Paul; Tang, Chiu C; Thompson, Stephen P; Parker, Julia E; Knowles, Jonathan C; Rehman, Ihtesham; Parkin, Ivan; Evans, Julian R G; Darr, Jawwad A

    2009-01-01

    A novel High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor was used to make directly and rapidly a 66-sample nanoparticle library (entire phase diagram) of nanocrystalline Ce(x)Zr(y)Y(z)O(2-delta) in less than 12 h. High resolution PXRD data were obtained for the entire heat-treated library (at 1000 degrees C/1 h) in less than a day using the new robotic beamline I11, located at Diamond Light Source (DLS). This allowed Rietveld-quality powder X-ray diffraction (PXRD) data collection of the entire 66-sample library in <1 day. Consequently, the authors rapidly mapped out phase behavior and sintering behaviors for the entire library. Out of the entire 66-sample heat-treated library, the PXRD data suggests that 43 possess the fluorite structure, of which 30 (out of 36) are ternary compositions. The speed, quantity and quality of data obtained by our new approach, offers an exciting new development which will allow structure-property relationships to be accessed for nanoceramics in much shorter time periods.

  1. MW-assisted synthesis of LiFePO 4 for high power applications

    Science.gov (United States)

    Beninati, Sabina; Damen, Libero; Mastragostino, Marina

    LiFePO 4/C was prepared by solid-state reaction from Li 3PO 4, Fe 3(PO 4) 2·8H 2O, carbon and glucose in a few minutes in a scientific MW (microwave) oven with temperature and power control. The material was characterized by X-ray diffraction, scanning electron microscopy and by TGA analysis to evaluate carbon content. The electrochemical characterization as positive electrode in EC (ethylene carbonate)-DMC (dimethylcarbonate) 1 M LiPF 6 was performed by galvanostatic charge-discharge cycles at C/10 to evaluate specific capacity and by sequences of 10 s discharge-charge pulses, at different high C-rates (5-45C) to evaluate pulse-specific power in simulate operative conditions for full-HEV application. The maximum pulse-specific power and, particularly, pulse efficiency values are quite high and make MW synthesis a very promising route for mass production of LiFePO 4/C for full-HEV batteries at low energy costs.

  2. Synthesis and studies of novel high metal content organic aerogels obtained from a polymerizable titanium complex

    International Nuclear Information System (INIS)

    Cadra, S.

    2010-01-01

    Inertial Confinement Fusion (ICF) is a technique widely studied by the French atomic commission (CEA). Experiments will be performed within the Laser Megajoule (LMJ). They require innovative materials like organic aerogels that constitute laser targets. Such polymeric material must provide both a high porosity and a significant titanium percentage (1 atom %). Moreover, the monomers developed must be compatible with the synthesis procedure already in use. According to these specifications, a new polymerizable titanium complex was synthesized and fully characterized. This air and moisture-stable monomer provides a high metal percentage. Its free-radical cross-linked copolymerization affords several titanium-containing polymers. These gels were dried under supercritical conditions and organic aerogels were obtained. The chemical compositions of these materials were investigated by NMR, IR and elemental analysis while their structure was characterized by MEB-EDS, MET, N 2 adsorption/desorption isotherms measurements and SAXS. The data collected fit the specification requirements. Moreover, the mechanisms responsible of the foam nano-structure formation were discussed. (author) [fr

  3. FPGA-Based Channel Coding Architectures for 5G Wireless Using High-Level Synthesis

    Directory of Open Access Journals (Sweden)

    Swapnil Mhaske

    2017-01-01

    Full Text Available We propose strategies to achieve a high-throughput FPGA architecture for quasi-cyclic low-density parity-check codes based on circulant-1 identity matrix construction. By splitting the node processing operation in the min-sum approximation algorithm, we achieve pipelining in the layered decoding schedule without utilizing additional hardware resources. High-level synthesis compilation is used to design and develop the architecture on the FPGA hardware platform. To validate this architecture, an IEEE 802.11n compliant 608 Mb/s decoder is implemented on the Xilinx Kintex-7 FPGA using the LabVIEW FPGA Compiler in the LabVIEW Communication System Design Suite. Architecture scalability was leveraged to accomplish a 2.48 Gb/s decoder on a single Xilinx Kintex-7 FPGA. Further, we present rapidly prototyped experimentation of an IEEE 802.16 compliant hybrid automatic repeat request system based on the efficient decoder architecture developed. In spite of the mixed nature of data processing—digital signal processing and finite-state machines—LabVIEW FPGA Compiler significantly reduced time to explore the system parameter space and to optimize in terms of error performance and resource utilization. A 4x improvement in the system throughput, relative to a CPU-based implementation, was achieved to measure the error-rate performance of the system over large, realistic data sets using accelerated, in-hardware simulation.

  4. Hydrothermal synthesis of highly nitrogen-doped few-layer graphene via solid–gas reaction

    International Nuclear Information System (INIS)

    Liang, Xianqing; Zhong, Jun; Shi, Yalin; Guo, Jin; Huang, Guolong; Hong, Caihao; Zhao, Yidong

    2015-01-01

    Highlights: • A novel approach to synthesis of N-doped few-layer graphene has been developed. • The high doping levels of N in products are achieved. • XPS and XANES results reveal a thermal transformation of N bonding configurations. • The developed method is cost-effective and eco-friendly. - Abstract: Nitrogen-doped (N-doped) graphene sheets with high doping concentration were facilely synthesized through solid–gas reaction of graphene oxide (GO) with ammonia vapor in a self-designed hydrothermal system. The morphology, surface chemistry and electronic structure of N-doped graphene sheets were investigated by TEM, AFM, XRD, XPS, XANES and Raman characterizations. Upon hydrothermal treatment, up to 13.22 at% of nitrogen could be introduced into the crumpled few-layer graphene sheets. Both XPS and XANES analysis reveal that the reaction between oxygen functional groups in GO and ammonia vapor produces amide and amine species in hydrothermally treated GO (HTGO). Subsequent thermal annealing of the resultant HTGO introduces a gradual transformation of nitrogen bonding configurations in graphene sheets from amine N to pyridinic and graphitic N with the increase of annealing temperature. This study provides a simple but cost-effective and eco-friendly method to prepare N-doped graphene materials in large-scale for potential applications

  5. Synthesis of high-quality diesel with furfural and 2-methylfuran from hemicellulose.

    Science.gov (United States)

    Li, Guangyi; Li, Ning; Wang, Zhiqiang; Li, Changzhi; Wang, Aiqin; Wang, Xiaodong; Cong, Yu; Zhang, Tao

    2012-10-01

    Hydroxyalkylation-alkylation (HAA) coupled with hydrodeoxygenation is a promising route for the synthesis of renewable high-quality diesel or jet fuel. In this work, a series of solid-acid catalysts were firstly used for HAA between lignocellulose-derived furan and carbonyl compounds. Among the investigated catalysts, Nafion-212 resin demonstrated the highest activity and stability. Owing to the high activity of the reactants and the advantage in industrial integration, the HAA of 2-methylfuran (2-MF) and furfural can be considered as a prospective route in future applications. Catalyst loading, reaction temperature, and time had evident effects on the HAA of 2-MF and furfural over Nafion-212 resin. Finally, the HAA product of 2-MF and furfural was hydrogenated over a Pd/C catalyst and hydrodeoxygenated over Pt-loaded solid-acid catalysts. Pt/zirconium phosphate (Pt/ZrP) was found to be the best catalyst for hydrodeoxygenation. Over the 4 % Pt/ZrP catalyst, a 94 % carbon yield of diesel and 75 % carbon yield of C15 hydrocarbons (with 6-butylundecane as the major component) was achieved. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Carbohydrate-Assisted Combustion Synthesis To Realize High-Performance Oxide Transistors.

    Science.gov (United States)

    Wang, Binghao; Zeng, Li; Huang, Wei; Melkonyan, Ferdinand S; Sheets, William C; Chi, Lifeng; Bedzyk, Michael J; Marks, Tobin J; Facchetti, Antonio

    2016-06-08

    Owing to high carrier mobilities, good environmental/thermal stability, excellent optical transparency, and compatibility with solution processing, thin-film transistors (TFTs) based on amorphous metal oxide semiconductors (AOSs) are promising alternatives to those based on amorphous silicon (a-Si:H) and low-temperature (IGZO) TFTs suffer from low carrier mobilities and/or inferior bias-stress stability versus their sputtered counterparts. Here we report that three types of environmentally benign carbohydrates (sorbitol, sucrose, and glucose) serve as especially efficient fuels for IGZO film combustion synthesis to yield high-performance TFTs. The results indicate that these carbohydrates assist the combustion process by lowering the ignition threshold temperature and, for optimal stoichiometries, enhancing the reaction enthalpy. IGZO TFT mobilities are increased to >8 cm(2) V(-1) s(-1) on SiO2/Si gate dielectrics with significantly improved bias-stress stability. The first correlations between precursor combustion enthalpy and a-MO densification/charge transport are established.

  7. Electrochemical synthesis of highly ordered polypyrrole on copper modified aluminium substrates

    International Nuclear Information System (INIS)

    Siddaramanna, Ashoka; Saleema, N.; Sarkar, D.K.

    2014-01-01

    Fabrication of highly ordered conducting polymers on metal surfaces has received a significant interest owing to their potential applications in organic electronic devices. In this context, we have developed a simple method for the synthesis of highly ordered polypyrrole (PPy) on copper modified aluminium surfaces via electrochemical polymerization process. A series of characteristic peaks of PPy evidenced on the infrared spectra of these surfaces confirm the formation of PPy. The X-ray diffraction (XRD) pattern of PPy deposited on copper modified aluminium surfaces also confirmed the deposition of PPy as a sharp and intense peak at 2θ angle of 23° attributable to PPy is observed while this peak is absent on PPy deposited on as-received aluminium surfaces. An atomic model of the interface of PPy/Cu has been presented based on the inter-atomic distance of copper–copper of (1 0 0) plane and the inter-monomer distance of PPy, to describe the ordering of PPy on Cu modified Al surfaces.

  8. Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Gordon Center for Integrated Science, 929 E. 57th Street, Chicago, Illinois 60637 (United States); Nash, P. [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Chen, X.Q.; Wei, P. [Materials processing Modeling Division, Shenyang National Laboratory for Materials Science, Institute of Metals Research, 72 Wenhua Road, Shenyang City (China)

    2015-06-05

    Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb{sub 3}Sc{sub 5}(−61.3 ± 2.9); PbTi{sub 4}(−16.6 ± 2.4); Pb{sub 3}Y{sub 5}(−64.8 ± 3.6); Pb{sub 3}Zr{sub 5}(−50.6 ± 3.1); PbNb{sub 3}(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd{sub 3}(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available.

  9. A high-throughput and quantitative method to assess the mutagenic potential of translesion DNA synthesis

    Science.gov (United States)

    Taggart, David J.; Camerlengo, Terry L.; Harrison, Jason K.; Sherrer, Shanen M.; Kshetry, Ajay K.; Taylor, John-Stephen; Huang, Kun; Suo, Zucai

    2013-01-01

    Cellular genomes are constantly damaged by endogenous and exogenous agents that covalently and structurally modify DNA to produce DNA lesions. Although most lesions are mended by various DNA repair pathways in vivo, a significant number of damage sites persist during genomic replication. Our understanding of the mutagenic outcomes derived from these unrepaired DNA lesions has been hindered by the low throughput of existing sequencing methods. Therefore, we have developed a cost-effective high-throughput short oligonucleotide sequencing assay that uses next-generation DNA sequencing technology for the assessment of the mutagenic profiles of translesion DNA synthesis catalyzed by any error-prone DNA polymerase. The vast amount of sequencing data produced were aligned and quantified by using our novel software. As an example, the high-throughput short oligonucleotide sequencing assay was used to analyze the types and frequencies of mutations upstream, downstream and at a site-specifically placed cis–syn thymidine–thymidine dimer generated individually by three lesion-bypass human Y-family DNA polymerases. PMID:23470999

  10. Synthesis, characterization, and cytotoxicity evaluation of high-magnetization multifunctional nanoclusters

    Energy Technology Data Exchange (ETDEWEB)

    Petran, Anca; Radu, Teodora; Nan, Alexandrina [National Institute for Research and Development of Isotopic and Molecular Technologies (Romania); Olteanu, Diana; Filip, Adriana, E-mail: adrianafilip33@yahoo.com; Clichici, Simona; Baldea, Ioana [Iuliu Hatieganu University of Medicine and Pharmacy, Department of Physiology (Romania); Suciu, Maria; Turcu, Rodica, E-mail: rodica.turcu@itim-cj.ro [National Institute for Research and Development of Isotopic and Molecular Technologies (Romania)

    2017-01-15

    The paper presents the synthesis, characterization, and in vitro cytotoxicity tests of Fe{sub 3}O{sub 4} magnetic nanoclusters coated with ethylenediaminetetraacetic acid disodium salt (EDTA). Electron microscopy analysis (SEM) evidences that magnetite nanoparticles are closely packed into the clusters stabilized with EDTA with well-defined near spherical shapes and sizes in the range 100–200 nm. From XRD measurements, we determined the mean size of the crystallites inside the magnetic cluster about 36 nm. The saturation magnetization determined for the magnetic clusters stabilized with EDTA has high value, about 81.7 emu/g at 300 K. X-ray photoelectron spectroscopy has been used to determine both the elemental and chemical structure of the magnetic cluster surface. In vitro studies have shown that the magnetic clusters at low doses did not induce toxicity on human umbilical vein endothelial cells or lesions of the cell membrane. In contrast, at high doses, the magnetic clusters increased the lipid peroxidation and reduced the leakage of a cytoplasmic enzyme, lactate dehydrogenase (LDH), in parallel with increasing the antioxidant defense.

  11. Synthesis of site-heterologous haptens for high-affinity anti-pyraclostrobin antibody generation.

    Science.gov (United States)

    Mercader, Josep V; Agulló, Consuelo; Abad-Somovilla, Antonio; Abad-Fuentes, Antonio

    2011-03-07

    The design and synthesis of functional chemical derivatives of small organic molecules is usually a key step for the intricate production of a variety of bioconjugates. In this respect, the derivatization site at which the spacer arm is introduced in immunizing conjugates constitutes a highly critical parameter for the generation of high-affinity and selective antibodies. However, due to the usual complexity of the required synthetic procedures, the appropriate comparison of alternative tethering positions has often been neglected. In the present study, meticulous strategies were followed to prepare synthetic derivatives of pyraclostrobin with the same linkers located at diverse rationally-chosen sites. Activity appraisal of antibodies and bioconjugates was carried out by bidimensional competitive direct and indirect immunoassays, and a superior performance of two of the three synthesized haptens was found. Finally, a detailed analysis of the conformations of the target molecule and the synthesized haptens in aqueous solution was done using computer assisted molecular modeling techniques. This study suggested that the lower titers and affinities of one set of antibodies are most probably due to conformational effects of the spacer arm in the immunizing bioconjugate.

  12. Methods of synthesis and performance improvement of lithium iron phosphate for high rate Li-ion batteries: A review

    Directory of Open Access Journals (Sweden)

    T.V.S.L. Satyavani

    2016-03-01

    Full Text Available Lithium ion battery technology has the potential to meet the requirements of high energy density and high power density applications. A continuous search for novel materials is pursued continually to exploit the latent potential of this technology. In this review paper, methods for preparation of Lithium Iron Phosphate are discussed which include solid state and solution based synthesis routes. The methods to improve the electrochemical performance of lithium iron phosphate are presented in detail.

  13. The rapid synthesis of high purity [{sup 18}F]butyrophenone neuroleptics from nitro precursors for PET study

    Energy Technology Data Exchange (ETDEWEB)

    Hashizume, Kazunari; Hashimoto, Naoto; Kato, Hiroo; Cork, D G; Miyake, Yoshihiro [National Cardiovascular Center, Suita, Osaka (Japan)

    1995-04-01

    We have completed rapid syntheses of [{sup 18}F]butyrophenone neuroleptics ([{sup 18}F]haloperidol and [{sup 18}F]spiperone) from their nitro precursors in high radiochemical yields (up to 21%) by combining a one-step nitro-fluoro exchange reaction and a novel high performance liquid chromatography (HPLC) separation method. The synthesis time was ca. 95 min and both the radiochemical and chemical purities of the labeled products were over 99%. (author).

  14. Acute high-caffeine exposure increases autophagic flux and reduces protein synthesis in C2C12 skeletal myotubes.

    Science.gov (United States)

    Hughes, M A; Downs, R M; Webb, G W; Crocker, C L; Kinsey, S T; Baumgarner, Bradley L

    2017-04-01

    Caffeine is a highly catabolic dietary stimulant. High caffeine concentrations (1-10 mM) have previously been shown to inhibit protein synthesis and increase protein degradation in various mammalian cell lines. The purpose of this study was to examine the effect of short-term caffeine exposure on cell signaling pathways that regulate protein metabolism in mammalian skeletal muscle cells. Fully differentiated C2C12 skeletal myotubes either received vehicle (DMSO) or 5 mM caffeine for 6 h. Our analysis revealed that caffeine promoted a 40% increase in autolysosome formation and a 25% increase in autophagic flux. In contrast, caffeine treatment did not significantly increase the expression of the skeletal muscle specific ubiquitin ligases MAFbx and MuRF1 or 20S proteasome activity. Caffeine treatment significantly reduced mTORC1 signaling, total protein synthesis and myotube diameter in a CaMKKβ/AMPK-dependent manner. Further, caffeine promoted a CaMKII-dependent increase in myostatin mRNA expression that did not significantly contribute to the caffeine-dependent reduction in protein synthesis. Our results indicate that short-term caffeine exposure significantly reduced skeletal myotube diameter by increasing autophagic flux and promoting a CaMKKβ/AMPK-dependent reduction in protein synthesis.

  15. NaCl as a solid solvent to assist the mechanochemical synthesis and post-synthesis of hierarchical porous MOFs with high I2 vapour uptake.

    Science.gov (United States)

    Yang, Junyi; Feng, Xiao; Lu, Guangnong; Li, Yulin; Mao, Chaochao; Wen, Zhongliang; Yuan, Wenbing

    2018-04-03

    The use of salts as grinding media to assist the mechanosynthesis, and the following one-pot mechanochemical post-synthesis, of hierarchically porous MOFs was carried out efficiently by ball milling. NaCl or KCl were used as a solid solvent to initially pre-grind with 1,3,5-benzenetricarboxylic acid (H3BTC) and copper acetate monhydrate, respectively, for 1 minute, then both mixtures were combined together for a further 20 minutes of grinding, and the resultant mixture was finally washed with ethanol and water to obtain the hierarchically micro-, meso- and macroporous HKUST-1 with a high yield. Moreover, the post-synthesis of these as-obtained hierarchically porous HKUST-1 was easily performed via grinding triethylenediamine (TED) with the above unwashed crude-products for 20 minutes. By adjusting the amount of NaCl and TED added, we simply fabricated the pore- and function-adjustable hierarchically porous HKUST-1. Furthermore, these as-obtained HKUST-1 products showed high performance in the capture of volatile iodine.

  16. Controlled synthesis of high-quality crystals of monolayer MoS2 for nanoelectronic device application

    DEFF Research Database (Denmark)

    Yang, Xiaonian; Li, Qiang; Hu, Guofeng

    2016-01-01

    . Monolayer MoS2 so far can be obtained by mechanical exfoliation or chemical vapor deposition (CVD). However, controllable synthesis of large area monolayer MoS2 with high quality needs to be improved and their growth mechanism requires more studies. Here we report a systematical study on controlled...... synthesis of high-quality monolayer MoS2 single crystals using low pressure CVD. Large-size monolayer MoS2 triangles with an edge length up to 405 mu m were successfully synthesized. The Raman and photoluminescence spectroscopy studies indicate high homogenous optical characteristic of the synthesized...... monolayer MoS2 triangles. The transmission electron microscopy results demonstrate that monolayer MoS2 triangles are single crystals. The back-gated field effect transistors (FETs) fabricated using the as-grown monolayer MoS2 show typical n-type semiconductor behaviors with carrier mobility up to 21.8 cm(2...

  17. Effects of Tobacco Taxation and Pricing on Smoking Behavior in High Risk Populations: A Knowledge Synthesis

    Directory of Open Access Journals (Sweden)

    David Boisclair

    2011-10-01

    Full Text Available Tobacco taxation is an essential component of a comprehensive tobacco control strategy. However, to fully realize the benefits it is vital to understand the impact of increased taxes among high-risk subpopulations. Are they influenced to the same extent as the general population? Do they need additional measures to influence smoking behavior? The objectives of this study were to synthesize the evidence regarding differential effects of taxation and price on smoking in: youth, young adults, persons of low socio-economic status, with dual diagnoses, heavy/long-term smokers, and Aboriginal people. Using a better practices approach, a knowledge synthesis was conducted using a systematic review of the literature and an expert advisory panel. Experts were involved in developing the study plan, discussing findings, developing policy recommendations, and identifying priorities for future research. Most studies found that raising cigarette prices through increased taxes is a highly effective measure for reducing smoking among youth, young adults, and persons of low socioeconomic status. However, there is a striking lack of evidence about the impact of increasing cigarette prices on smoking behavior in heavy/long-term smokers, persons with a dual diagnosis and Aboriginals. Given their high prevalence of smoking, urgent attention is needed to develop effective policies for the six subpopulations reviewed. These findings will be of value to policy-makers and researchers in their efforts to improve the effectiveness of tobacco control measures, especially with subpopulations at most risk. Although specific studies are needed, tobacco taxation is a key policy measure for driving success.

  18. Synthesis of high saturation magnetic iron oxide nanomaterials via low temperature hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Bhavani, P.; Rajababu, C.H. [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India); Arif, M.D. [Environmental Magnetism Laboratory, Indian Institute of Geomagnetism (IIG), Navi Mumbai 410218, Mumbai (India); Reddy, I. Venkata Subba [Department of Physics, Gitam University, Hyderabad Campus, Rudraram, Medak 502329 (India); Reddy, N. Ramamanohar, E-mail: manoharphd@gmail.com [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India)

    2017-03-15

    Iron oxide nanoparticles (IONPs) were synthesized through a simple low temperature hydrothermal approach to obtain with high saturation magnetization properties. Two series of iron precursors (sulfates and chlorides) were used in synthesis process by varying the reaction temperature at a constant pH. The X-ray diffraction pattern indicates the inverse spinel structure of the synthesized IONPs. The Field emission scanning electron microscopy and high resolution transmission electron microscopy studies revealed that the particles prepared using iron sulfate were consisting a mixer of spherical (16–40 nm) and rod (diameter ~20–25 nm, length <100 nm) morphologies that synthesized at 130 °C, while the IONPs synthesized by iron chlorides are found to be well distributed spherical shapes with size range 5–20 nm. On other hand, the IONPs synthesized at reaction temperature of 190 °C has spherical (16–46 nm) morphology in both series. The band gap values of IONPs were calculated from the obtained optical absorption spectra of the samples. The IONPs synthesized using iron sulfate at temperature of 130 °C exhibited high saturation magnetization (M{sub S}) of 103.017 emu/g and low remanant magnetization (M{sub r}) of 0.22 emu/g with coercivity (H{sub c}) of 70.9 Oe{sub ,} which may be attributed to the smaller magnetic domains (d{sub m}) and dead magnetic layer thickness (t). - Highlights: • Comparison of iron oxide materials prepared with Fe{sup +2}/Fe{sup +3} sulfates and chlorides at different temperatures. • We prepared super-paramagnetic and soft ferromagnetic magnetite nanoparticles. • We report higher saturation magnetization with lower coercivity.

  19. Effects of tobacco taxation and pricing on smoking behavior in high risk populations: a knowledge synthesis.

    Science.gov (United States)

    Bader, Pearl; Boisclair, David; Ferrence, Roberta

    2011-11-01

    Tobacco taxation is an essential component of a comprehensive tobacco control strategy. However, to fully realize the benefits it is vital to understand the impact of increased taxes among high-risk subpopulations. Are they influenced to the same extent as the general population? Do they need additional measures to influence smoking behavior? The objectives of this study were to synthesize the evidence regarding differential effects of taxation and price on smoking in: youth, young adults, persons of low socio-economic status, with dual diagnoses, heavy/long-term smokers, and Aboriginal people. Using a better practices approach, a knowledge synthesis was conducted using a systematic review of the literature and an expert advisory panel. Experts were involved in developing the study plan, discussing findings, developing policy recommendations, and identifying priorities for future research. Most studies found that raising cigarette prices through increased taxes is a highly effective measure for reducing smoking among youth, young adults, and persons of low socioeconomic status. However, there is a striking lack of evidence about the impact of increasing cigarette prices on smoking behavior in heavy/long-term smokers, persons with a dual diagnosis and Aboriginals. Given their high prevalence of smoking, urgent attention is needed to develop effective policies for the six subpopulations reviewed. These findings will be of value to policy-makers and researchers in their efforts to improve the effectiveness of tobacco control measures, especially with subpopulations at most risk. Although specific studies are needed, tobacco taxation is a key policy measure for driving success.

  20. Abridged acid-base wet-milling synthesis of high purity hydroyapatite

    Directory of Open Access Journals (Sweden)

    Sandi Carolina Ruiz-Mendoza

    2008-06-01

    Full Text Available There is a plethora of routes to produce hydroxyapatite(HA and in general calcium phosphates(CP but production usually leads to a mixture of several phases. Besides ionic contamination, most of these methods are cumbersome, restricted to small volumes of product and require a lot of thermal energy. The acid-base route eliminates foreign ions or additives and its only byproduct is water. Heterogeneous reaction drawback is that solid reactants do not easily come in contact with each other and therefore addition and stirring times become very lengthy and still the product is a mixture. The synthesis started from calcium hydroxide and phosphoric acid (PA. Ball milling was used to favor kinetics and stoichiometry. Six sets of PA addition, paddle stirring and ball milling times were used. Products were evaluated by X ray diffraction (XRD, Fourier Transform Infrared (FTIR, scanning electron microscopy (SEM, X ray fluorescence (XRF and Ca/P ratio. Chemical analysis for calcium proceeded through oxalate precipitate and phosphorus by the phosphomolibdate technique. A set of conditions yielding high purity HA was established.

  1. Synthesis, characterization and magnetic properties of highly monodispersed PtNi nanoparticles

    International Nuclear Information System (INIS)

    Du, Juan-Juan; Yang, Yi; Zhang, Rong-Hua; Zhou, Xin-Wen

    2015-01-01

    In this paper, we report the controlled-synthesis of PtNi nanoparticles through galvanic displacement reaction and chemical reduction. The size, composition and morphology of the products are characterized by transmission electron microscopy (TEM), powder X-ray diffraction (XRD), energy dispersed X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analyses. The structure and composition of the PtNi nanoparticles can be controlled by adjusting the synthetic conditions. The possible formation mechanism is obtained from the academic analysis and experimental studies. The results of the magnetic measurement illustrate that the PtNi nanoparticles show a superparamagnetic behavior with a blocking temperature (T B ) about 8.0 K. - Highlights: • Highly monodispersed PtNi nanoparticles were synthesized by galvanic displacement reaction. • The formation of Pt nanocrystals was the foremost step because of its self-catalysis effect. • The PtNi nanoparticles show a superparamagnetic behavior with a T B about 8.0 K

  2. Synthesis and characterization of ruthenium fluorides and oxide fluorides with high oxidation states

    International Nuclear Information System (INIS)

    Meublat, L.

    1989-10-01

    The synthesis of ruthenium fluorides and oxide fluorides with high oxidation states was attempted from dioxide RuO 2 and tetroxide RuO 4 . Three fluorinating agents were used: fluorine, chlorine trifluoride and krypton difluoride. The reactions were achieved in anhydrous hydrogen fluoride at room temperature. Thus, the reaction of RuO 4 with CIF 3 enabled us to prepare chloryl hexafluororuthenate (V), CIO 2 + RuF 6 - , a new compound well identified by vibrational spectroscopy (infra-red and Raman), the structure of which was determined. The reaction of KrF 2 with RuO 4 gave the oxide tetrafluoride RuOF 4 , the previously published syntheses and properties of which were not in agreement with each other. This compound was definitely characterized here by chemical analysis, infra-red spectroscopy and X-ray powder diffraction. The product of thermal decomposition (70 0 C) of RuOF 4 is presumably RuF 4 since only oxygen is liberated during this decomposition. At last, the reaction of KrF 2 with RuO 2 probably leads to the formation of the new oxide fluoride RuO 2 F 4 . Indeed, no oxygen is given off during this reaction, the chemical analysis of the red-orange coloured solid residue is almost in agreement with the one proposed and its infra-red absorption spectrum indicates the presence of ruthenium-oxygen and ruthenium-terminal and bridging fluorine bonds [fr

  3. Synthesis and characterization of ruthenium fluorides and oxide fluorides with high oxidation states

    International Nuclear Information System (INIS)

    Meublat, L.

    1989-01-01

    The synthesis of ruthenium fluorides and oxide fluorides with high oxidation states was attempted from dioxide RuO 2 and tetroxide RuO 4 . Three fluorinating agents were used: fluorine, chlorine trifluoride and krypton difluoride. The reactions were achieved in anhydrous hydrogen fluoride at room temperature. Thus, the reaction of RuO 4 with CIF 3 enabled us to prepare chloryl hexafluororuthenate (V), ClO 2 + RuF 6 - , a new compound well idendified by vibrational spectroscopy (infra-red and Raman), the structure of which was determined. The reaction of KrF 2 with RuO 4 gave the oxide tetrafluoride RuOF 4 , the previously published syntheses and properties of which were not in agreement with each other. This compound was definitely characterized here by chemical analysis, infra-red spectroscopy and X-ray powder diffraction. The product of thermal decomposition (70 0 C) of RuOF 4 is presumably RuF 4 since only oxygen is liberated during this decomposition. At last, the reaction of KrF 2 with RuO 2 probably leads to the formation of the new oxide fluoride RuO 2 F 4 . Indeed, no oxygen is given off during this reaction, the chemical analysis of the red-orange coloured solid residue is almost in agreement with the one proposed and its infra-red absorption spectrum indicates the presence of ruthenium-oxygen and ruthenium-terminal and bridging fluorine bonds [fr

  4. Synthesis and characterization of a highly stable dendritic catechol-tripod bearing technetium-99m

    International Nuclear Information System (INIS)

    Bertin, A.; Gallani, J.L.; Felder-Flesch, D.; Michou-Gallani, A.I.; Steibel, J.

    2010-01-01

    The synthesis and preliminary biological tests (in vitro toxicity, in vitro stability) of new Tc(III)-radiolabelled dendro-chelates are presented. A dendritic 99m Tc chelate 1 derived from a pre-organized tripodal tris-catechol-amide exhibits a kinetic stability by far more important than its corresponding diethylenetriamine pentaacetic acid (DTPA) homologue 2. This permitted an assessment of the real impact of the pre-organized tripodal structure on kinetic inertness (and thus toxicity), an important issue to address when considering in vivo applications. Radiolabelling was performed using the stannous chloride reduction method; while DTPA-homologue 2 showed a high radiolabelling efficiency (96% radiolabelling yield after 30 min), tripodal complex 1 induced a 93% complexation yield after 45 min. In contrast, radio-complex 1 derived from the most rigid and organized structure has a higher kinetic stability than 2. Indeed, while dissociation of 2 reached 50% after 1 h 30 min in physiological media like phosphate buffer saline (PBS) and bovine serum albumin (BSA), over 80% of 1 remained stable during the half-life of the radionuclide (6.02 h for 99m Tc). Measurements of the cell leakage resulting from membrane damage of neuronal cells treated with increasing concentrations of dendritic ligand 16, together with pictures of treated neurons after staining, showed no detectable toxicity. (authors)

  5. Synthesis and new structure shaping mechanism of silica particles formed at high pH

    International Nuclear Information System (INIS)

    Zhang, Henan; Zhao, Yu; Akins, Daniel L.

    2012-01-01

    For the sol–gel synthesis of silica particles under high pH catalytic conditions (pH>12) in water/ethanol solvent, we have deduced that the competing dynamics of chemical etching and sol–gel process can explain the types of silica particles formed and their morphologies. We have demonstrated that emulsion droplets that are generated by adding tetraethyl orthosilicate (TEOS) to a water–ethanol solution serve as soft templates for hollow spherical silica (1–2 μm). And if the emulsion is converted by the sol–gel process, one finds that suspended solid silica spheres of diameter of ∼900 nm are formed. Moreover, several other factors are found to play fundamental roles in determining the final morphologies of silica particles, such as by variation of the pH (in our case, using OH – ) to a level where condensation dominates; by changing the volume ratios of water/ethanol; and using an emulsifier (specifically, CTAB) - Graphical abstract: “Local chemical etching” and sol–gel process have been proposed to interpret the control of morphologies of silica particles through varying initial pHs in syntheses. Highlights: ► Different initial pHs in our syntheses provides morphological control of silica particles. ► “Local chemical etching” and sol–gel process describes the formation of silica spheres. ► The formation of emulsions generates hollow silica particles.

  6. Synthesis of Highly Stable Cobalt Nanomaterial Using Gallic Acid and Its Application in Catalysis

    Directory of Open Access Journals (Sweden)

    Saba Naz

    2014-01-01

    Full Text Available We report the room temperature (25–30°C green synthesis of cobalt nanomaterial (CoNM in an aqueous medium using gallic acid as a reducing and stabilizing agent. pH 9.5 was found to favour the formation of well dispersed flower shaped CoNM. The optimization of various parameters in preparation of nanoscale was studied. The AFM, SEM, EDX, and XRD characterization studies provide detailed information about synthesized CoNM which were of 4–9 nm in dimensions. The highly stable CoNM were used to study their catalytic activity for removal of azo dyes by selecting methyl orange as a model compound. The results revealed that 0.4 mg of CoNM has shown 100% removal of dye from 50 μM aqueous solution of methyl orange. The synthesized CoNM can be easily recovered and recycled several times without decrease in their efficiency.

  7. High-yield water-based synthesis of truncated silver nanocubes

    International Nuclear Information System (INIS)

    Chang, Yun-Min; Lu, I-Te; Chen, Chih-Yuan; Hsieh, Yu-Chi; Wu, Pu-Wei

    2014-01-01

    Highlights: • Development of a water-based formula to fabricate truncated Ag nanocubes. • The sample exhibits (1 0 0), (1 1 0), and (1 1 1) on the facets, edges, and corners. • The sample shows three characteristic absorption peaks due to plasma resonance. -- Abstract: A high-yield water-based hydrothermal synthesis was developed using silver nitrate, ammonia, glucose, and cetyltrimethylammonium bromide (CTAB) as precursors to synthesize truncated silver nanocubes with uniform sizes and in large quantities. With a fixed CTAB concentration, truncated silver nanocubes with sizes of 49.3 ± 4.1 nm were produced when the molar ratio of glucose/silver cation was maintained at 0.1. The sample exhibited (1 0 0), (1 1 0), and (1 1 1) planes on the facets, edges, and corners, respectively. In contrast, with a slightly larger glucose/silver cation ratio of 0.35, well-defined nanocubes with sizes of 70.9 ± 3.8 nm sizes were observed with the (1 0 0) plane on six facets. When the ratio was further increased to 1.5, excess reduction of silver cations facilitated the simultaneous formation of nanoparticles with cubic, spherical, and irregular shapes. Consistent results were obtained from transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and UV–visible absorption measurements

  8. High-yield water-based synthesis of truncated silver nanocubes

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Yun-Min; Lu, I-Te; Chen, Chih-Yuan; Hsieh, Yu-Chi; Wu, Pu-Wei, E-mail: ppwu@mail.nctu.edu.tw

    2014-02-15

    Highlights: • Development of a water-based formula to fabricate truncated Ag nanocubes. • The sample exhibits (1 0 0), (1 1 0), and (1 1 1) on the facets, edges, and corners. • The sample shows three characteristic absorption peaks due to plasma resonance. -- Abstract: A high-yield water-based hydrothermal synthesis was developed using silver nitrate, ammonia, glucose, and cetyltrimethylammonium bromide (CTAB) as precursors to synthesize truncated silver nanocubes with uniform sizes and in large quantities. With a fixed CTAB concentration, truncated silver nanocubes with sizes of 49.3 ± 4.1 nm were produced when the molar ratio of glucose/silver cation was maintained at 0.1. The sample exhibited (1 0 0), (1 1 0), and (1 1 1) planes on the facets, edges, and corners, respectively. In contrast, with a slightly larger glucose/silver cation ratio of 0.35, well-defined nanocubes with sizes of 70.9 ± 3.8 nm sizes were observed with the (1 0 0) plane on six facets. When the ratio was further increased to 1.5, excess reduction of silver cations facilitated the simultaneous formation of nanoparticles with cubic, spherical, and irregular shapes. Consistent results were obtained from transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and UV–visible absorption measurements.

  9. Discovery of earth-abundant nitride semiconductors by computational screening and high-pressure synthesis

    Science.gov (United States)

    Hinuma, Yoyo; Hatakeyama, Taisuke; Kumagai, Yu; Burton, Lee A.; Sato, Hikaru; Muraba, Yoshinori; Iimura, Soshi; Hiramatsu, Hidenori; Tanaka, Isao; Hosono, Hideo; Oba, Fumiyasu

    2016-01-01

    Nitride semiconductors are attractive because they can be environmentally benign, comprised of abundant elements and possess favourable electronic properties. However, those currently commercialized are mostly limited to gallium nitride and its alloys, despite the rich composition space of nitrides. Here we report the screening of ternary zinc nitride semiconductors using first-principles calculations of electronic structure, stability and dopability. This approach identifies as-yet-unreported CaZn2N2 that has earth-abundant components, smaller carrier effective masses than gallium nitride and a tunable direct bandgap suited for light emission and harvesting. High-pressure synthesis realizes this phase, verifying the predicted crystal structure and band-edge red photoluminescence. In total, we propose 21 promising systems, including Ca2ZnN2, Ba2ZnN2 and Zn2PN3, which have not been reported as semiconductors previously. Given the variety in bandgaps of the identified compounds, the present study expands the potential suitability of nitride semiconductors for a broader range of electronic, optoelectronic and photovoltaic applications. PMID:27325228

  10. Microwave Synthesis and Magnetic Properties of High Tc Superconductor MGB2

    International Nuclear Information System (INIS)

    Koeseoglu, Y.

    2004-01-01

    Polycrystalline powders of MgB 2 have been synthesized by microwave synthesis technique. Crystallographic information of the sample was investigated by powder X-ray diffraction (XRD). The main phase was determined as MgB2, and secondary phases as MgB4 and MgO. The temperature dependence of magnetic properties of polycrystalline MgB2, synthesized by using microwave heating of the constituents have been characterized by SQUID magnetometer and X-band EPR spectrometer. The transition temperature to the superconducting phase is observed as 39K for both measurements. An isotropic, strong and very narrow EPR signal corresponding to free electron g-value (ge=2.0023) is observed. The observed line broadening with decreasing temperature might arise from the dipolar interactions between the superparamagnetic nanoparticles. Normally, the internal magnetic field originating from magnetic entities is expected to be more uniform as a result of highly ordered magnetic moments at low temperatures; giving narrower ESR line in contrary in our case. While the ESR line is broadened, the signal intensity is drastically decreased just below T c =39 K corresponding to a transition temperature from normal to superconducting state. Some minor changes in both intensity and line width curves might be taken as signs for changes of local crystalline field symmetry around weakly localized conduction electrons or holes, which are the sources of ESR signal in MgB 2 compound

  11. Synthesis by irradiation and mechanism and structural characterization study of high melt strength polypropylene

    International Nuclear Information System (INIS)

    Lugao, Ademar Benevolo

    2004-01-01

    Polypropylene molecular structure is made only by linear molecules interacting by weak forces. The resulting PP has very low melt strength (MS). MS is important to make feasible to process PP by all the transformation technologies based on the free expansion of the melt. The aim of this work was to develop a new process to synthesize PP with crosslinks and/or long chain branches, known as High Melt Strength Polypropylene (HMSPP) and to characterize its structure and synthesis mechanism. HMSPP was obtained by the irradiation of PP under a crosslinking (acetylene) atmosphere or inert or oxidative one, followed by thermal treatment for radical recombination and thermal treatment for annihilation of the remaining radicals under reactive or inert atmosphere. The results from rheological characterization showed that the highest levels of MS were obtained by conducting irradiation and thermal treatments under crosslinking atmospheres. The results for the elucidation of reaction mechanism by electron spin resonance (ESR) showed that acetylene irradiation is effective in promoting the creation of double bonds, based on the formation of polyenil radicals. The results of structural unraveling showed that radiation promotes predominantly the degradation of atactic molecules or molecules with atactic defects. These results support the hypothesis of formation of branched PP molecules based on the reaction of those fragments with the double bonds created in the PP molecules. (author)

  12. Synthesis, characterization, and in vitro biological evaluation of highly stable diversely functionalized superparamagnetic iron oxide nanoparticles

    International Nuclear Information System (INIS)

    Bhattacharya, Dipsikha; Sahu, Sumanta K.; Banerjee, Indranil; Das, Manasmita; Mishra, Debashish; Maiti, Tapas K.; Pramanik, Panchanan

    2011-01-01

    In this article, we report the design and synthesis of a series of well-dispersed superparamagnetic iron oxide nanoparticles (SPIONs) using chitosan as a surface modifying agent to develop a potential T 2 contrast probe for magnetic resonance imaging (MRI). The amine, carboxyl, hydroxyl, and thiol functionalities were introduced on chitosan-coated magnetic probe via simple reactions with small reactive organic molecules to afford a series of biofunctionalized nanoparticles. Physico-chemical characterizations of these functionalized nanoparticles were performed by TEM, XRD, DLS, FTIR, and VSM. The colloidal stability of these functionalized iron oxide nanoparticles was investigated in presence of phosphate buffer saline, high salt concentrations and different cell media for 1 week. MRI analysis of human cervical carcinoma (HeLa) cell lines treated with nanoparticles elucidated that the amine-functionalized nanoparticles exhibited higher amount of signal darkening and lower T 2 relaxation in comparison to the others. The cellular internalization efficacy of these functionalized SPIONs was also investigated with HeLa cancer cell line by magnetically activated cell sorting (MACS) and fluorescence microscopy and results established selectively higher internalization efficacy of amine-functionalized nanoparticles to cancer cells. These positive attributes demonstrated that these nanoconjugates can be used as a promising platform for further in vitro and in vivo biological evaluations.

  13. Synthesis, Characterizations, and Applications of Metal-Ions Incorporated High Quality MCM-41 Catalysts

    International Nuclear Information System (INIS)

    Lim, Steven S.; Haller, Gary L.

    2013-01-01

    Various metal ions (transition and base metals) incorporated MCM-41 catalysts can be synthesized using colloidal and soluble silica with non-sodium involved process. Transition metal ion-typically V 5+ , Co 2+ , and Ni 2+ -incorporated MCM-41 catalysts were synthesized by isomorphous substitution of Si ions in the framework. Each incorporated metal ion created a single species in the silica framework, single-site solid catalyst, showing a substantial stability in reduction and catalytic activity. Radius of pore curvature effect was investigated with Co-MCM-41 by temperature programmed reduction (TPR). The size of metallic Co clusters, sub-nanometer, could be controlled by a proper reduction treatment of Co-MCM-41 having different pore size and the initial pH adjustment of the Co-MCM-41 synthesis solution. These small metallic clusters showed a high stability under a harsh reaction condition without serious migration, resulting from a direct anchoring of small metallic clusters to the partially or unreduced metal ions on the surface. After a complete reduction, partial occlusion of the metallic cluster surface by amorphous silica stabilized the particles against aggregations. As a probe reaction of particle size sensitivity, carbon single wall nanotubes (SWNT) were synthesized using Co-MCM-41. A metallic cluster stability test was performed by CO methanation using Co- and Ni-MCM-41. Methanol and methane partial oxidations were carried out with V-MCM-41, and the radius of pore curvature effect on the catalytic activity was investigated

  14. Characterization of ceramics and intermetallics fabricated by self-propagating high-temperature synthesis

    International Nuclear Information System (INIS)

    Hurst, J.B.

    1989-05-01

    Three efforts aimed at investigating the process of self-propagating high temperature synthesis (SHS) for the fabrication of structural ceramics and intermetallics are summarized. Of special interest was the influence of processing variables such as exothermic dopants, gravity, and green state morphology in materials produced by SHS. In the first effort directed toward the fabrication of SiC, exothermic dopants of yttrium and zirconium were added to SiO2 or SiO2 + NiO plus carbon powder mix and processed by SHS. This approach was unsuccessful since it did not produce the desired product of crystalline SiC. In the second effort, the influence of gravity was investigated by examining Ni-Al microstructures which were produced by SHS combustion waves traveling with and opposite the gravity direction. Although final composition and total porosities of the combusted Ni-Al compounds were found to be gravity independent, larger pores were created in those specimens which were combusted opposite to the gravity force direction. Finally, it was found that green microstructure has a significant effect on the appearance of the combusted piece. Severe pressing laminations were observed to arrest the combustion front for TiC samples

  15. Prolonged Adaptation to a Low or High Protein Diet Does Not Modulate Basal Muscle Protein Synthesis Rates - A Substudy.

    Science.gov (United States)

    Hursel, Rick; Martens, Eveline A P; Gonnissen, Hanne K J; Hamer, Henrike M; Senden, Joan M G; van Loon, Luc J C; Westerterp-Plantenga, Margriet S

    2015-01-01

    Based on controlled 36 h experiments a higher dietary protein intake causes a positive protein balance and a negative fat balance. A positive net protein balance may support fat free mass accrual. However, few data are available on the impact of more prolonged changes in habitual protein intake on whole-body protein metabolism and basal muscle protein synthesis rates. To assess changes in whole-body protein turnover and basal muscle protein synthesis rates following 12 weeks of adaptation to a low versus high dietary protein intake. A randomized parallel study was performed in 40 subjects who followed either a high protein (2.4 g protein/kg/d) or low protein (0.4 g protein/kg/d) energy-balanced diet (30/35/35% or 5/60/35% energy from protein/carbohydrate/fat) for a period of 12 weeks. A subgroup of 7 men and 8 women (body mass index: 22.8±2.3 kg/m2, age: 24.3±4.9 y) were selected to evaluate the impact of prolonged adaptation to either a high or low protein intake on whole body protein metabolism and basal muscle protein synthesis rates. After the diet, subjects received continuous infusions with L-[ring-2H5]phenylalanine and L-[ring-2H2]tyrosine in an overnight fasted state, with blood samples and muscle biopsies being collected to assess post-absorptive whole-body protein turnover and muscle protein synthesis rates in vivo in humans. After 12 weeks of intervention, whole-body protein balance in the fasted state was more negative in the high protein treatment when compared with the low protein treatment (-4.1±0.5 vs -2.7±0.6 μmol phenylalanine/kg/h;Pprotein breakdown (43.0±4.4 vs 37.8±3.8 μmol phenylalanine/kg/h;Psynthesis (38.9±4.2 vs 35.1±3.6 μmol phenylalanine/kg/h;Pprotein group. Basal muscle protein synthesis rates were maintained on a low vs high protein diet (0.042±0.01 vs 0.045±0.01%/h;P = 0.620). In the overnight fasted state, adaptation to a low-protein intake (0.4 g/kg/d) does not result in a more negative whole-body protein balance and

  16. Synthesis, characterization and spectral properties of new, highly fluorescent, 4-hydroxythiazoles

    Czech Academy of Sciences Publication Activity Database

    Kammel, R.; Tarabová, D.; Machalický, O.; Nepraš, M.; Frumarová, Božena; Hanusek, J.

    2016-01-01

    Roč. 128, May (2016), s. 101-110 ISSN 0143-7208 Institutional support: RVO:61389013 Keywords : 4-hydroxythiazoles * synthesis * absorption spectra Subject RIV: CC - Organic Chemistry Impact factor: 3.473, year: 2016

  17. Effects of high energy ball milling on synthesis and characteristics of Ti-Mg alloys

    CSIR Research Space (South Africa)

    Chikwanda, HK

    2008-01-01

    Full Text Available The synthesis of Ti-Mg alloys using mechanical alloying method has been investigated. Effects of the mechanical alloying parameters on the resultant microstructural features have been studied. This work presents the effects of milling speed...

  18. Cyclopropanes and hypervalent iodine reagents: high energy compounds for applications in synthesis and catalysis.

    Science.gov (United States)

    Fernández González, Davinia; De Simone, Filippo; Brand, Jonathan P; Nicolai, Stefano; Waser, Jérôme

    2011-01-01

    One of the major challenges faced by organic chemistry is the efficient synthesis of increasingly complex molecules. Since October 2007, the Laboratory of Catalysis and Organic Synthesis (LCSO) at EPFL has been working on the development of catalytic reactions based on the Umpolung of the innate reactivity of functional groups. Electrophilic acetylene synthons have been developed using the exceptional properties of ethynyl benziodoxolone (EBX) hypervalent iodine reagents for the alkynylation of heterocycles and olefins. The obtained acetylenes are important building blocks for organic chemistry, material sciences and chemical biology. The ring-strain energy of donor-acceptor cyclopropanes was then used in the first catalytic formal homo-Nazarov cyclization. In the case of aminocyclopropanes, the method could be applied in the synthesis of the alkaloids aspidospermidine and goniomitine. The developed methods are expected to have a broad potential for the synthesis and functionalization of complex organic molecules, including carbocycles and heterocycles.

  19. A practical synthesis of a gamma-secretase inhibitor.

    Science.gov (United States)

    Scott, Jeremy P; Lieberman, David R; Beureux, Olivier M; Brands, Karel M J; Davies, Antony J; Gibson, Andrew W; Hammond, Deborah C; McWilliams, Chris J; Stewart, Gavin W; Wilson, Robert D; Dolling, Ulf-H

    2007-05-25

    A practical and scaleable synthesis of the gamma-secretase inhibitor 1 is reported. The inhibitor consists of a central trisubstituted cyclohexane core with appended propionic acid, 2,5-difluorophenyl, and 4-chlorophenylsulfonyl moieties. Two alternative synthetic strategies, proceeding by way of a common disubstituted cyclohexanone derivative 5, were studied. In the preferred route, conjugate reduction of acrylonitrile derivative 4 with L-Selectride configures the desired relative stereochemistry of the cyclohexane core with >99.9:0.1 dr. A second strategy, based on catalyst-controlled hydrogenation of racemic cyclohexene derivative 2, is more convergent but less diastereoselective (up to 75:25 dr). The common cyclohexanone intermediate 5 was constructed by a regioselective Diels-Alder condensation of a 1,1-disubstituted vinyl sulfone 6 with 2-trimethylsiloxybutadiene.

  20. Bromide (Br) - Based Synthesis of Ag Nanocubes with High-Yield

    OpenAIRE

    Wu, Fan; Wang, Wenhui; Xu, Zhongfeng; Li, Fuli

    2015-01-01

    The geometry of metal nanoparticles greatly affects the properties of the localized surface plasmon resonance and surface-enhanced Raman scattering. The synthesis of metal nanoparticles with controllable geometry has thus attracted extensive attentions. In this work, we report a modified polyol synthesis approach of silver (Ag) nanocubes through tuning the concentration of bromide ions (Br? ions). We have systematically investigated the effect of Br? ions in the polyol process, and find that ...

  1. Preparation of high temperature superconductor ceramics using cuban reactives. Optimization of the synthesis method

    International Nuclear Information System (INIS)

    Leyva Fabelo, A.; Cruz, C.; Aragon, B.; Suarez, J.C.; Mora, M.

    1991-01-01

    Results of the crystallographic characterization of a group of Cuban Products, which are evaluated to be employed in HTSC fabrication are presented in this paper. The first results on the synthesis of HTSC (RBa 2 Cu 3 0 7δ , R= Y, La, Nd) using Cuban reactives, are presented. The so called 'solid state reaction method of synthesis' was optimized, obtaining a critical temperature of more than 93 k

  2. New labeling methods via organometallic species: new synthesis of a chiral methyl group

    International Nuclear Information System (INIS)

    Faucher, Nicolas

    2000-01-01

    Chapter 1: New labeling methods via organometallic species. In the first part of this work, we have developed a new labeling strategy based on the hydrogenolysis of organolithium compounds with tritium gas or deuterium gas. This reaction is catalyzed with palladium on charcoal and leads to the labelled compounds with direct replacement of the proton by its isotopes ("2H or "3H) without further chemical modification of the target molecule. Using this strategy, tritium or deuterium atoms can be introduced in a region but also in a stereoselective fashion with more than 90% ee. The former result was obtained using (-)-sparteine during the lithiation step. Chapter II: New synthesis of a chiral methyl group. In the second part of this work, we have developed a new synthetic method to prepare chiral ditosyl-methylamine using 4,5-disubstituted oxazolidines. Dia-stereoselective substitution of the methoxy group of a 2-alkoxy-oxazolidine by a deuteride in the presence of a Lewis acid leads to the 2-deutero-oxazolidine in a highly stereoselective fashion (de = 100%). Still using a lewis acid, a tritiated hydride open the former 2-deutero-oxazolidine to afford chiral methyl group borne by the nitrogen. Further de-protection and re-protection steps lead to the ditosyl-methylamine with an ee of 65% (RIS= 83/17). Nowadays, this is the best known synthetic method, not only in terms of enantioselectivity but also in terms of chemical yield and number of radioactive steps. As NTs_2 is a fairly good leaving group, the ditosyl-methylamine offers the possibility of introducing chiral methyl group in many substrates using a S_N2 reaction with various nucleophiles. This last point leads to many potential applications in the field of biochemistry or for mechanical studies. (author) [fr

  3. Effects of Fuel to Synthesis of CaTiO3 by Solution Combustion Synthesis for High-Level Nuclear Waste Ceramics.

    Science.gov (United States)

    Jung, Choong-Hwan; Kim, Yeon-Ku; Han, Young-Min; Lee, Sang-Jin

    2016-02-01

    A solution combustion process for the synthesis of perovskite (CaTiO3) powders is described. Perovskite is one of the crystalline host matrics for the disposal of high-level radioactive wastes (HLW) because it immobilizes Sr and Lns elements by forming solid solutions. Solution combustion synthesis, which is a self-sustaining oxi-reduction reaction between nitrate and organic fuel, the exothermic reaction, and the heat evolved convert the precursors into their corresponding oxide products above 1100 degrees C in air. To investigate the effects of amino acid on the combustion reaction, various types of fuels were used; a glycine, amine and carboxylic ligand mixture. Sr, La and Gd-nitrate with equivalent amounts of up to 20% of CaTiO3 were mixed with Ca and Ti nitrate and amino acid. X-ray diffraction analysis, SEM and TEM were conducted to confirm the formed phases and morphologies. While powders with an uncontrolled shape are obtained through a general oxide-route process, Ca(Sr, Lns)TiO3 powders with micro-sized soft agglomerates consisting of nano-sized primary particles can be prepared using this method.

  4. Α-amino-β-fluorocyclopropanecarboxylic acids as a new tool for drug development: synthesis of glutamic acid analogs and agonist activity towards metabotropic glutamate receptor 4.

    Science.gov (United States)

    Lemonnier, Gérald; Lion, Cédric; Quirion, Jean-Charles; Pin, Jean-Philippe; Goudet, Cyril; Jubault, Philippe

    2012-08-01

    Herein we describe the diastereoselective synthesis of glutamic acid analogs and the evaluation of their agonist activity towards metabotropic glutamate receptor subtype 4 (mGluR4). These analogs are based on a monofluorinated cyclopropane core substituted with an α-aminoacid function. The potential of this new building block as a tool for the development of a novel class of drugs is demonstrated with racemic analog 11a that displayed the best agonist activity with an EC50 of 340 nM. Copyright © 2012 Elsevier Ltd. All rights reserved.

  5. Synthesis of partially graphitic ordered mesoporous carbons with high surface areas

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Wenjun; Wan, Ying [Department of Chemistry, Key Laboratory of Resource Chemistry of Ministry of Education, Shanghai Normal University, Shanghai 200234 (China); Dou, Yuqian; Zhao, Dongyuan [Department of Chemistry, Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Fudan University, Shanghai 200433 (China)

    2011-01-01

    Graphitic carbons with ordered mesostructure and high surface areas (of great interest in applications such as energy storage) have been synthesized by a direct triblock-copolymer-templating method. Pluronic F127 is used as a structure-directing agent, with a low-molecular-weight phenolic resol as a carbon source, ferric oxide as a catalyst, and silica as an additive. Inorganic oxides can be completely eliminated from the carbon. Small-angle XRD and N{sub 2} sorption analysis show that the resultant carbon materials possess an ordered 2D hexagonal mesostructure, uniform bimodal mesopores (about 1.5 and 6 nm), high surface area ({proportional_to}1300 m{sup 2}/g), and large pore volumes ({proportional_to}1.50 cm{sup 3}/g) after low-temperature pyrolysis (900 C). All surface areas come from mesopores. Wide-angle XRD patterns demonstrate that the presence of the ferric oxide catalyst and the silica additive lead to a marked enhancement of graphitic ordering in the framework. Raman spectra provide evidence of the increased content of graphitic sp{sup 2} carbon structures. Transmission electron microscopy images confirm that numerous domains in the ordered mesostructures are composed of characteristic graphitic carbon nanostructures. The evolution of the graphitic structure is dependent on the temperature and the concentrations of the silica additive, and ferric oxide catalyst. Electrochemical measurements performed on this graphitic mesoporous carbon when used as an electrode material for an electrochemical double layer capacitor shows rectangular-shaped cyclic voltammetry curves over a wide range of scan rates, even up to 200 mV/s, with a large capacitance of 155 F/g in KOH electrolyte. This method can be widely applied to the synthesis of graphitized carbon nanostructures. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  6. Metallic oxide nano-clusters synthesis by ion implantation in high purity Fe10Cr alloy

    International Nuclear Information System (INIS)

    Zheng, Ce

    2015-01-01

    ODS (Oxide Dispersed Strengthened) steels, which are reinforced with metal dispersions of nano-oxides (based on Y, Ti and O elements), are promising materials for future nuclear reactors. The detailed understanding of the mechanisms involved in the precipitation of these nano-oxides would improve manufacturing and mechanical properties of these ODS steels, with a strong economic impact for their industrialization. To experimentally study these mechanisms, an analytical approach by ion implantation is used, to control various parameters of synthesis of these precipitates as the temperature and concentration. This study demonstrated the feasibility of this method and concerned the behaviour of alloys models (based on aluminium oxide) under thermal annealing. High purity Fe-10Cr alloys were implanted with Al and O ions at room temperature. Transmission electron microscopy observations showed that the nano-oxides appear in the Fe-10Cr matrix upon ion implantation at room temperature without subsequent annealing. The mobility of implanted elements is caused by the defects created during ion implantation, allowing the nucleation of these nanoparticles, of a few nm in diameter. These nanoparticles are composed of aluminium and oxygen, and also chromium. The high-resolution experiments show that their crystallographic structure is that of a non-equilibrium compound of aluminium oxide (cubic γ-Al 2 O 3 type). The heat treatment performed after implantation induces the growth of the nano-sized oxides, and a phase change that tends to balance to the equilibrium structure (hexagonal α-Al 2 O 3 type). These results on model alloys are fully applicable to industrial materials: indeed ion implantation reproduces the conditions of milling and heat treatments are at equivalent temperatures to those of thermo-mechanical treatments. A mechanism involving the precipitation of nano-oxide dispersed in ODS alloys is proposed in this manuscript based on the obtained experimental results

  7. Synthesis of highly active and dual-functional electrocatalysts for methanol oxidation and oxygen reduction reactions

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Qi; Zhang, Geng; Xu, Guangran; Li, Yingjun [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Liu, Baocang [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Inner Mongolia Key Lab of Nanoscience and Nanotechnology, Inner Mongolia University, Hohhot 010021 (China); Gong, Xia [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Zheng, Dafang [State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012 (China); Zhang, Jun [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Inner Mongolia Key Lab of Nanoscience and Nanotechnology, Inner Mongolia University, Hohhot 010021 (China); Wang, Qin, E-mail: qinwang@imu.edu.cn [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Inner Mongolia Key Lab of Nanoscience and Nanotechnology, Inner Mongolia University, Hohhot 010021 (China)

    2016-12-15

    Graphical abstract: Ternary RuMPt (M = Fe, Co, Ni, and Cu) nanodendrities (NDs) catalysts, are successfully synthesized by using a facile method. The as-obtained ternary catalysts manifest superior catalytic activity and stability both in terms of surface and mass specific activities toward the methanol oxidation and oxygen reduction reactions, as compared to the binary catalysts and the commercial Pt/C catalysts. - Highlights: • Ternary RuMPt catalysts are synthesized by using a facile method. • The catalysts manifest superior catalytic activity towards the MOR and ORR. • High activities are attributed to enhanced electron density and synergistic effects. - Abstract: The promising Pt-based ternary catalyst is crucial for polymer electrolyte membrane fuel cells (PEMFCs) due to improving catalytic activity and durability for both methanol oxidation reaction and oxygen reduction reaction. In this work, a facile strategy is used for the synthesis ternary RuMPt (M = Fe, Co, Ni, and Cu) nanodendrities catalysts. The ternary RuMPt alloys exhibit enhanced specific and mass activity, positive half-wave potential, and long-term stability, compared with binary Pt-based alloy and the commercial Pt/C catalyst, which is attributed to the high electron density and upshifting of the d-band center for Pt atoms, and synergistic catalytic effects among Pt, M, and Ru atoms by introducing a transition metal. Impressively, the ternary RuCoPt catalyst exhibits superior mass activity (801.59 mA mg{sup −1}) and positive half-wave potential (0.857 V vs. RHE) towards MOR and ORR, respectively. Thus, the RuMPt nanocomposite is a very promising material to be used as dual electrocatalyst in the application of PEMFCs.

  8. Mechanically activated self-propagated high-temperature synthesis of nanometer-structured MgB2

    International Nuclear Information System (INIS)

    Radev, D.D.; Marinov, M.; Tumbalev, V.; Radev, I.; Konstantinov, L.

    2005-01-01

    Nanometer-sized MgB 2 was prepared via a two-step modification of the mechanically activated self-propagated high-temperature synthesis. The experimental conditions and some structural and phase characteristics of the synthesized product are reported. It is shown that a single-phase material can be prepared after 2 h of intense mechanical treatment of the starting magnesium and boron powders and a synthesis induced at a current-pulse density of 30 A cm -2 . The average size of MgB 2 particles synthesized in this way is 70-80 nm. It is also shown that using the same reagents and the 'classic' high-temperature interaction at 850 deg C with a protective atmosphere of pure Ar, mean particle size of the MgB 2 obtained is 50 μm

  9. The synthesis of amphipathic prodrugs of 1,2-diol drugs with saccharide conjugates by high regioselective enzymatic protocol.

    Science.gov (United States)

    Quan, Jing; Chen, Zhichun; Han, Chengyou; Lin, Xianfu

    2007-02-15

    A facile, high regioselective enzymatic synthesis approach for the preparation of amphipathic prodrugs with saccharides of mephenesin and chlorphenesin was developed. Firstly, transesterification of two drugs with divinyl dicarboxylates with different carbon chain length was performed under the catalysis of Candida antarctica lipase acrylic resin and Lipozyme in anhydrous acetone at 50 degrees C, respectively. A series of lipophilic derivatives with vinyl groups of mephenesin and chlorphenesin were prepared. The influences of different organic solvents, enzyme sources, reaction time, and the acylation reagents on the synthesis of vinyl esters were investigated. And then, protease-catalyzed high regioselective acylation of D-glucose and D-mannose with vinyl esters of mephenesin and chlorphenesin gave drug-saccharide derivatives in good yields. The studies of lipophilicity and hydrolysis in vitro of prodrugs verified that drug-saccharide derivatives had amphipathic properties, and both lipophilic and amphipathic drug derivatives had obvious controlled release characteristics.

  10. Size Tunable Synthesis of Highly Crystalline BaTiO3 Nanoparticles using Salt-Assisted Spray Pyrolysis

    International Nuclear Information System (INIS)

    Itoh, Yoshifumi; Lenggoro, I. Wuled; Okuyama, Kikuo; Maedler, Lutz; Pratsinis, Sotiris E.

    2003-01-01

    Highly crystalline, dense BaTiO 3 nanoparticles in a size range from 30 to 360nm with a narrow size distribution (σ g = 1.2-1.4) were prepared at various synthesis temperatures using a salt-assisted spray pyrolysis (SASP) method without the need for post-annealing. The effect of synthesis temperature on particle size, crystallinity and surface morphology of the nanoparticles were characterized by X-ray diffraction and scanning/transmission electron microscopy. The nature of the crystalline structure was analyzed by Rietveld refinement and Raman spectroscopy. The particle size decreased with decreasing operation temperature. The crystal phase was transformed from tetragonal to cubic at a particles size of about 50nm at room temperature. SASP can be used to produce high weight fraction of tetragonal BaTiO 3 nanoparticles down to 64nm in a single step

  11. Highly Stereoselective Intermolecular Haloetherification and Haloesterification of Allyl Amides

    Science.gov (United States)

    Soltanzadeh, Bardia; Jaganathan, Arvind; Staples, Richard J.

    2016-01-01

    An organocatalytic and highly regio-, diastereo-, and enantioselective intermolecular haloetherification and haloesterification reaction of allyl amides is reported. A variety of alkene substituents and substitution patterns are compatible with this chemistry. Notably, electronically unbiased alkene substrates exhibit exquisite regio- and diastereoselectivity for the title transformation. We also demonstrate that the same catalytic system can be used in both chlorination and bromination reactions of allyl amides with a variety of nucleophiles with little or no modification. PMID:26110812

  12. Solid-phase synthesis and structural characterization of highly substituted hydroxyproline-based 2,5-diketopiperazines

    DEFF Research Database (Denmark)

    Bianco; Sonksen; Roepstorff

    2000-01-01

    . The synthesis procedures were conceived to enable a sequence of Hyp alkylation, Hyp N-acylation, cyclization, and amide bond alkylation. Up to three different centers of molecular diversity were introduced around the DKP scaffold. Highly functionalized bicyclic compounds were obtained in good yield and purity...... with multidimensional NMR experiments. The described reaction pathways can be applied to the identification of heterocyclic molecule inhibitors to diverse enzyme targets....

  13. Highly Convergent Total Synthesis of (+)-Lithospermic Acid via a Late-Stage Intermolecular C–H Olefination

    Science.gov (United States)

    Wang, Dong-Hui; Yu, Jin-Quan

    2011-01-01

    The total synthesis of (+)-lithospermic acid is reported, which exploits two successive C–H activation reactions as the key steps. Rh-catalyzed carbene C–H insertion reaction using Davies’ catalyst built the dihydrobenzofuran core, and a late-stage intermolecular C–H olefination coupled the olefin unit with the dihydrobenzofuran core to construct the molecule in a highly convergent manner. PMID:21443224

  14. Gold nanoparticles supported on titanium dioxide: an efficient catalyst for highly selective synthesis of benzoxazoles and benzimidazoles.

    Science.gov (United States)

    Tang, Lin; Guo, Xuefeng; Yang, Yu; Zha, Zhenggen; Wang, Zhiyong

    2014-06-11

    A highly efficient and selective reaction for the synthesis of 2-substituted benzoxazoles and benzimidazoles catalyzed by Au/TiO2 has been developed via two hydrogen-transfer processes. This reaction has a good tolerance to air and water, a wide substrate scope, and represents a new avenue for practical C-N and C-O bond formation. More importantly, no additional additives, oxidants and reductants are required for the reaction and the catalyst can be recovered and reused readily.

  15. The Evolution of Chemical High-Throughput Experimentation To Address Challenging Problems in Pharmaceutical Synthesis.

    Science.gov (United States)

    Krska, Shane W; DiRocco, Daniel A; Dreher, Spencer D; Shevlin, Michael

    2017-12-19

    The structural complexity of pharmaceuticals presents a significant challenge to modern catalysis. Many published methods that work well on simple substrates often fail when attempts are made to apply them to complex drug intermediates. The use of high-throughput experimentation (HTE) techniques offers a means to overcome this fundamental challenge by facilitating the rational exploration of large arrays of catalysts and reaction conditions in a time- and material-efficient manner. Initial forays into the use of HTE in our laboratories for solving chemistry problems centered around screening of chiral precious-metal catalysts for homogeneous asymmetric hydrogenation. The success of these early efforts in developing efficient catalytic steps for late-stage development programs motivated the desire to increase the scope of this approach to encompass other high-value catalytic chemistries. Doing so, however, required significant advances in reactor and workflow design and automation to enable the effective assembly and agitation of arrays of heterogeneous reaction mixtures and retention of volatile solvents under a wide range of temperatures. Associated innovations in high-throughput analytical chemistry techniques greatly increased the efficiency and reliability of these methods. These evolved HTE techniques have been utilized extensively to develop highly innovative catalysis solutions to the most challenging problems in large-scale pharmaceutical synthesis. Starting with Pd- and Cu-catalyzed cross-coupling chemistry, subsequent efforts expanded to other valuable modern synthetic transformations such as chiral phase-transfer catalysis, photoredox catalysis, and C-H functionalization. As our experience and confidence in HTE techniques matured, we envisioned their application beyond problems in process chemistry to address the needs of medicinal chemists. Here the problem of reaction generality is felt most acutely, and HTE approaches should prove broadly enabling

  16. Experimental synthesis of crystalline matrices based on Ce, Ba, Sr zirconates for immobilization of high-level radioactive actinides

    International Nuclear Information System (INIS)

    Anderson, E.B.; Burakov, B.E.; Vasiliev, V.G.; Starchenko, V.A.

    1993-01-01

    In geological disposal of high-level radioactive waste the main storage barriers, in the first place the matrix containing radionuclides, must remain undestructible over a long period of time. Very high requirements are imposed for the matrices from the viewpoint of their chemical stability and mechanical strength. Zirconates may be classified among compounds potentially suitable for the creation of crystalline matrices incorporating radionuclides in their structure. The paper considers results of laboratory experiments on the synthesis of crystalline matrices based on various zirconates by the methods of gas-static and axial pressing. Problems are discussed concerning the crystalline matrix industrial synthesis technology developed at the Radium Institute. One of the most promising directions in solving the problem of high-level waste (HLW) removal from the sphere of human activity is disposal in deep geological formations. The realization of this direction envisages creation of multibarrier compositions. Special attention is paid to the technology for the synthesis of the first, the most crucial, engineering barrier: the matrix into which radionuclides are incorporated. It is assumed that crystalline compounds best satisfy all the requirements as the most thermodynamically stable

  17. Synthesis of high quality single-walled carbon nanotubes via a catalytic layer reinforced by self-assembled monolayers

    International Nuclear Information System (INIS)

    Adhikari, Prashanta Dhoj; Song, Wooseok; Cha, Myoung-Jun; Park, Chong-Yun

    2013-01-01

    This work reports the synthesis of high quality single-walled carbon nanotubes (SWCNT) using a catalytic layer reinforced by self-assembled monolayers (SAM). Amine-SAM was introduced on a SiO 2 /Si substrate and then an iron nanoparticles solution was dropped on the substrate by spin-coating. This catalytic template was used to grow carbon nanotubes by chemical vapor deposition and the synthesized SWCNT were observed to be prominent, based on the size distribution. Highly dense SWCNT with a diameter of about 1.1-1.2 nm were produced at 800-850 °C. Moreover, the diameter distribution of the SWCNT was more selective at a growth temperature of 900 °C. These findings provide important insights for a SAM support layer that can play the role as a restriction for the agglomeration of iron catalyst and is promising for the synthesis of high quality SWCNT. - Highlights: • Fe nanoparticles on self-assembled monolayers (SAM) containing template is underlined. • Its catalytic behavior to synthesis single-walled carbon nanotubes is studied. • The role of SAM on catalytic template is explored

  18. Synthesis and spectroscopic behavior of highly luminescent Eu 3+-dibenzoylmethanate (DBM) complexes with sulfoxide ligands

    Science.gov (United States)

    Niyama, E.; Brito, H. F.; Cremona, M.; Teotonio, E. E. S.; Reyes, R.; Brito, G. E. S.; Felinto, M. C. F. C.

    2005-09-01

    In this paper the synthesis, characterization and photoluminescent behavior of the [RE(DBM) 3L 2] complexes (RE = Gd and Eu) with a variety of sulfoxide ligands; L = benzyl sulfoxide (DBSO), methyl sulfoxide (DMSO), phenyl sulfoxide (DPSO) and p-tolyl sulfoxide (PTSO) have been investigated in solid state. The emission spectra of the Eu 3+-β-diketonate complexes show characteristics narrow bands arising from the 5D 0 → 7F J ( J = 0-4) transitions, which are split according to the selection rule for C n, C nv or C s site symmetries. The experimental Judd-Ofelt intensity parameters ( Ω2 and Ω4), radiative ( Arad) and non-radiative ( Anrad) decay rates, and R02 for the europium complexes have been determined and compared. The highest value of Ω2 (61.9 × 10 -20 cm 2) was obtained to the complex with PTSO ligand, indicating that Eu 3+ ion is in the highly polarizable chemical environment. The higher values of the experimental quantum yield ( q) and emission quantum efficiency of the emitter 5D 0 level ( η) for the Eu-complexes with DMSO, DBSO and PTSO sulfoxides suggest that these complexes are promising Light Conversion Molecular Devices (LCMDs). The lower value of quantum yield ( q = 1%), for the hydrated complex [Eu(DBM) 3(H 2O)], indicates that the luminescence quenching occurs via multiphonon relaxation by coupling with the OH-oscillators from water molecule coordinated to rare earth ion. The pure red emission of the Eu-complexes has been confirmed by ( x, y) color coordinates.

  19. The thermochemical behavior of some binary shape memory alloys by high temperature direct synthesis calorimetry

    International Nuclear Information System (INIS)

    Meschel, S.V.; Pavlu, J.; Nash, P.

    2011-01-01

    Research highlights: → We studied 14 shape memory alloys. → The enthalpies of formation and structure characteristics are summarized. → Theoretical predictions by ab initio calculations compare better with experimental measurements than Miedema's semi empirical model. - Abstract: The standard enthalpies of formation of some shape memory alloys have been measured by high temperature direct synthesis calorimetry at 1373 K. The following results (in kJ/mol of atoms) are reported: CoCr (-0.3 ± 2.9); CuMn (-3.7 ± 3.2); Cu 3 Sn (-10.4 ± 3.1); Fe 2 Tb (-5.5 ± 2.4); Fe 2 Dy (-1.6 ± 2.9); Fe 17 Tb 2 (-2.1 ± 3.1); Fe 17 Dy 2 (-5.3 ± 1.7); FePd 3 (-16.0 ± 2.7); FePt (-23.0 ± 1.9); FePt 3 (-20.7 ± 2.3); NiMn (-24.9 ± 2.6); TiNi (-32.7 ± 1.0); TiPd (-60.3 ± 2.5). The results are compared with some earlier experimental values obtained by calorimetry and by EMF technique. They are also compared with predicted values on the basis of the semi empirical model of Miedema and co-workers and with ab initio calculations when available. We will also assess the available information regarding the structures of these alloys.

  20. Study on synthesis of ultrafine Cu–Ag core–shell powders with high electrical conductivity

    International Nuclear Information System (INIS)

    Peng Yuhsien; Yang Chihhao; Chen Kuanting; Popuri, Srinivasa R.; Lee, Ching-Hwa; Tang, Bo-Shin

    2012-01-01

    Highlights: ► This synthesis method is relatively facile, novel and eco-friendly. ► Toxic agents were not used for chelating agent, reductant or dispersant in our method. ► The reaction can under room temperature for energy saving purpose. ► Cu–Ag core–shell powders with homogeneous cover-silver layer. ► The resistivity of Cu–Ag core–shell powders has the same value as the pure silver. - Abstract: Cu–Ag composite powders with high electrical conductivity were synthesized by electroless plating of silver sulfate, copper powders with eco-friendly sodium citrate as reducing agent, dispersant and chelating agent in an aqueous system. The influences of sodium citrate/Ag ratio on Ag coatings of Cu powders were investigated. Ag was formed a dense coating on the surface of Cu powders at a molar ratio of sodium citrate/Ag = 0.07/1. SEM showed an uniformity of Ag coatings on Cu powders. SEM-EDX also revealed that Cu cores were covered by Ag shells on the whole. The surface composition analysis by XPS indicated that without Cu or Ag atoms in the surface were oxidized. The resistivity measurements of Cu–Ag paste shows that they have closer resistivity as the pure silver paste's after 250 °C for 30 min heat-treatment (2.55 × 10 −4 Ω cm) and 350 °C for 30 min heat-treatment (1.425 × 10 −4 Ω cm).

  1. Establishing a high yielding streptomyces-based cell-free protein synthesis system.

    Science.gov (United States)

    Li, Jian; Wang, He; Kwon, Yong-Chan; Jewett, Michael C

    2017-06-01

    Cell-free protein synthesis (CFPS) has emerged as a powerful platform for applied biotechnology and synthetic biology, with a range of applications in synthesizing proteins, evolving proteins, and prototyping genetic circuits. To expand the current CFPS repertoire, we report here the development and optimization of a Streptomyces-based CFPS system for the expression of GC-rich genes. By developing a streamlined crude extract preparation protocol and optimizing reaction conditions, we were able to achieve active enhanced green fluorescent protein (EGFP) yields of greater than 50 μg/mL with batch reactions lasting up to 3 h. By adopting a semi-continuous reaction format, the EGFP yield could be increased to 282 ± 8 μg/mL and the reaction time was extended to 48 h. Notably, our extract preparation procedures were robust to multiple Streptomyces lividans and Streptomyces coelicolor strains, although expression yields varied. We show that our optimized Streptomyces lividans system provides benefits when compared to an Escherichia coli-based CFPS system for increasing percent soluble protein expression for four Streptomyces-originated high GC-content genes that are involved in biosynthesis of the nonribosomal peptides tambromycin and valinomycin. Looking forward, we believe that our Streptomyces-based CFPS system will contribute significantly towards efforts to express complex natural product gene clusters (e.g., nonribosomal peptides and polyketides), providing a new avenue for obtaining and studying natural product biosynthesis pathways. Biotechnol. Bioeng. 2017;114: 1343-1353. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

  2. Chemical synthesis of highly stable PVA/PANI films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Patil, D.S.; Shaikh, J.S.; Dalavi, D.S.; Kalagi, S.S. [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Patil, P.S., E-mail: psp_phy@unishivaji.ac.in [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2011-08-15

    Highlights: {yields} Chemical synthesis of PVA/PANI films by spin and dip coating at room temperature. {yields} Thickness dependent supercapacitor behavior of PVA/PANI film. {yields} The synthesized film are highly stable up to 20,000 cycles. - Abstract: Polyvinyl alcohol (PVA)/polyaniline (PANI) thin films were chemically synthesized by adopting two step process: initially a thin layer (200 nm) of PVA was spin coated by using an aqueous PVA solution onto fluorine doped tin oxide (FTO) coated glass substrate, afterwards PANI was chemically polymerized from aniline monomer and dip coated onto the precoated substrate. The thickness of PANI layer was varied from 293 nm to 2367 nm by varying deposition cycles onto the precoated PVA thin film. The resultant PVA/PANI films were characterized for their optical, morphological and electrochemical properties. The FT-IR and Raman spectra revealed characteristic features of the PANI phase. The SEM study showed porous spongy structure. Electrochemical properties were studied by electrochemical impedance measurement and cyclic voltammetry. The electrochemical performance of PVA/PANI thin films was investigated in 1 M H{sub 2}SO{sub 4} aqueous electrolyte. The highest specific capacitance of 571 Fg{sup -1} was observed for the optimized thickness of 880 nm. The film was found to be stable for more than 20,000 cycles. The samples degraded slightly (25% decrement in specific capacitance) for the first 10,000 cycles. The degradation becomes much slower (10.8% decrement in specific capacitance) beyond 10,000 cycles. This dramatic improvement in the electrochemical stability of the PANI samples, without sacrificing specific capacitance was attributed to the optimized PVA layer.

  3. Synthesis and spectroscopic behavior of highly luminescent trinuclear europium complexes with tris-β-diketone ligand

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Dunjia, E-mail: dunjiawang@163.com; Pi, Yan; Liu, Hua; Wei, Xianhong; Hu, Yanjun; Zheng, Jing

    2014-11-15

    Highlights: • Synthesis of the tris-β-diketone ligand and its trinuclear europium complexes. • Photoluminescence behavior of trinuclear europium complexes. • Analysis of the Judd–Ofelt intensity parameters (Ω{sub t}), lifetime (τ) and quantum yield (η). - Abstract: A new tris-β-diketone ligand, 2-[4,6-bis-(1-benzoyl-2-oxo-2-phenyl-ethyl)-[1,3,5]triazin-2-yl] -1,3-diphenyl-propane-1,3-dione (H{sub 3}L), and its trinuclear europium complexes, Eu{sub 3}(DBM){sub 6}L (C1), Eu{sub 3}(DBM){sub 6}(Bipy){sub 3}L (C2) and Eu{sub 3}(DBM){sub 6}(Phen){sub 3}L (C3) were synthesized and their spectroscopic behaviors were studied by FT-IR, {sup 1}H NMR, UV–vis and photoluminescence spectroscopic techniques. These europium complexes exhibited the characteristic emission bands that arise from the {sup 5}D{sub 0} → {sup 7}F{sub J} (J = 0–4) transitions of the europium ion in solid state. The Ω{sub 2} and Ω{sub 4} intensity parameters, lifetime (τ) and luminescence quantum yield (η) were calculated according to the emission spectra and luminescence decay curves in solid state. The results indicated that these trinuclear europium complexes displayed a longer lifetime (τ) and higher luminescence quantum efficiency (η), especially complexes C2 (τ = 0.820 ms, η = 46.5%) and C3 (τ = 0.804 ms, η = 47.4%), which due to the effect of two additional europium ion lumophors and the introduction of the third ligands, Bipy or Phen in trinuclear complexes. Their Ω{sub 2} values demonstrated that the europium ion in these complexes is in a highly polarizable chemical environment.

  4. Synthesis of high quality diamond film for the dosimeter realization in the radiotherapy domain

    International Nuclear Information System (INIS)

    Vaissiere, Nicolas

    2014-01-01

    This thesis aims to master the MPCVD synthesis of heteroepitaxial diamond films of high crystalline quality on iridium substrate for radiotherapy dosimeters. This objective has led us to develop the epitaxial iridium layer grown on SrTiO 3 substrates (001). A vacuum frame equipped with an electron gun has been developed and calibrated. The obtained layers characterized by XRD, possess a structural quality equivalent to the state of the art/in literature. Bias Enhanced Nucleation (BEN)- MPCVD induces nucleation of 'domains' on the iridium surface, according a unique nucleation pathway. Significant work has been conducted on (BEN)-MPCVD optimization to obtain a reliable and reproducible method for generating homogeneous 'domains' on a surface of 5 x 5 mm 2 . Combined characterizations (SEM, XPS, AES) of 'domains' surface enabled us to establish the identity card of their chemical and morphological properties. We demonstrate that they contain diamond nuclei. In addition, the temporal expansion of these 'domains' seems to follow preferential directions <110> of iridium lattice during the (BEN)-MPCVD stage. From these results, self-supported heteroepitaxial diamond films 100μ-m thick have been grown. The correlation between their crystalline quality and their detection response was conducted with the LCD dosimeter team. The inhomogeneities in the crystal structure due to structural defects have been identified. To study more locally these samples, a measurement campaign was carried out by microbeam X on the DIFFABS line at Soleil Synchrotron. The combination of the different knowledge acquired during this thesis has allowed the fabrication and characterization of the first detector based on heteroepitaxial diamond at the LCD laboratory. (author) [fr

  5. Microstructure evolution of Mo–Si–Al system during self-propagation high-temperature synthesis

    International Nuclear Information System (INIS)

    Jia, Lei; Xie, Hui; Lu, Zhen-lin; Zhang, Chao

    2013-01-01

    Highlights: ► Phase transformation subsequence of the reaction system was given by a sketch. ► Transformation of MoSi 2 to Mo(Si, Al) 2 phase was observed by XRD analysis. ► Variation of diffraction peaks was discussed by lattice parameters calculation. -- Abstract: The microstructure and phase constitution of Mo(Si 1−x , Al x ) 2 alloys (x = 0.03, 0.1 and 0.4) prepared by self-propagation high-temperature synthesis is first investigated using SEM, EDS and XRD analysis. Then the lattice parameters and adiabatic temperature are calculated. Based on the above experimental and calculated results, the variation mechanism of diffraction peaks and phase transformation subsequence of the Mo–MoO 3 –Si–Al powders is discussed. Results show that, when the self-propagation reaction is over, there are a homogeneous Mo–Si–Al alloy melt and a fused Al 2 O 3 with lower density at top. Subsequently, MoSi 2 or Mo(Si, Al) 2 phase nucleates and grows as a primary phase in the Mo–Si–Al alloy melts, and then Al, Si substances are generated from the intergranular residual Al–Si liquid according to Al–Si binary phase diagram. The Al increase in the starting powder mixtures leads to the Al concentration increase in the Mo–Si–Al alloy melt. Consequently, MoSi 2 is transformed to Mo(Si, Al) 2 to phase in which Si is replaced by Al atoms and Al substance in the intergranular zones increased accordingly

  6. A scalable synthesis of highly stable and water dispersible Ag 44(SR)30 nanoclusters

    KAUST Repository

    AbdulHalim, Lina G.; Ashraf, Sumaira; Katsiev, Khabiboulakh; Kirmani, Ahmad R.; Kothalawala, Nuwan; Anjum, Dalaver H.; Abbas, Sikandar Zameer; Amassian, Aram; Stellacci, Francesco; Dass, Amala; Hussain, Irshad; Bakr, Osman

    2013-01-01

    We report the synthesis of atomically monodisperse thiol-protected silver nanoclusters [Ag44(SR)30] m, (SR = 5-mercapto-2-nitrobenzoic acid) in which the product nanocluster is highly stable in contrast to previous preparation methods. The method is one-pot, scalable, and produces nanoclusters that are stable in aqueous solution for at least 9 months at room temperature under ambient conditions, with very little degradation to their unique UV-Vis optical absorption spectrum. The composition, size, and monodispersity were determined by electrospray ionization mass spectrometry and analytical ultracentrifugation. The produced nanoclusters are likely to be in a superatom charge-state of m = 4-, due to the fact that their optical absorption spectrum shares most of the unique features of the intense and broadly absorbing nanoparticles identified as [Ag44(SR) 30]4- by Harkness et al. (Nanoscale, 2012, 4, 4269). A protocol to transfer the nanoclusters to organic solvents is also described. Using the disperse nanoclusters in organic media, we fabricated solid-state films of [Ag44(SR)30]m that retained all the distinct features of the optical absorption spectrum of the nanoclusters in solution. The films were studied by X-ray diffraction and photoelectron spectroscopy in order to investigate their crystallinity, atomic composition and valence band structure. The stability, scalability, and the film fabrication method demonstrated in this work pave the way towards the crystallization of [Ag44(SR)30]m and its full structural determination by single crystal X-ray diffraction. Moreover, due to their unique and attractive optical properties with multiple optical transitions, we anticipate these clusters to find practical applications in light-harvesting, such as photovoltaics and photocatalysis, which have been hindered so far by the instability of previous generations of the cluster. © 2013 The Royal Society of Chemistry.

  7. Knorr-Rabe partial reduction of pyrroles: Application to the synthesis of indolizidine alkaloids

    Directory of Open Access Journals (Sweden)

    Ryan John H

    2008-01-01

    Full Text Available Abstract Background The Birch reduction of electron rich pyrroles does not occur readily. However, dissolving metal reduction with zinc under acidic conditions gives 3-pyrrolines (2,5-dihydropyrroles in reasonable yield. This dissolving metal reduction was first reported by Knorr and Rabe in 1901 but since then has only been reported for the reduction of electron rich pyrroles. Results The partial reduction of bicyclic α-ketopyrrole derivatives has been performed under dissolving metal conditions with zinc and hydrochloric acid to give excellent yields of hexahydroindolizidines. This reduction method has been utilised for the diastereoselective synthesis of 5-alkylindolizidines and the stereoselectivity obtained is opposite to that of catalytic hydrogenation. Conclusion An efficient stereoselective synthesis of indolizidine alkaloids has been developed from α-ketopyrrole intermediates using a modified version of Knorr and Rabe's pyrrole reduction.

  8. Study of composite adsorbent synthesis and characterization for the removal of Cs in the high-salt and high-radioactive wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jimin; Lee, Keun Young; Kim, Kwang Wook; Lee, Eil Hee; Chung, Dong Yong; Moon, Jei Kwon [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Hyun, Jae Hyuk [Chungnam National University, Daejeon (Korea, Republic of)

    2017-03-15

    For the removal of cesium (Cs) from high radioactive/high salt-laden liquid waste, this study synthesized a highly efficient composite adsorbent (potassium cobalt ferrocyanide (PCFC)-loaded chabazite (CHA)) and evaluated its applicability. The composite adsorbent used CHA, which could accommodate Cs as well as other molecules, as a supporting material and was synthesized by immobilizing the PCFC in the pores of CHA through stepwise impregnation/precipitation with CoCl{sub 2} and K{sub 4}Fe (CN){sub 6} solutions. When CHA, with average particle size of more than 10 μm, is used in synthesizing the composite adsorbent, the PCFC particles were immobilized in a stable form. Also, the physical stability of the composite adsorbent was improved by optimizing the washing methodology to increase the purity of the composite adsorbent during the synthesis. The composite adsorbent obtained from the optimal synthesis showed a high adsorption rate of Cs in both fresh water (salt-free condition) and seawater (high-salt condition), and had a relatively high value of distribution coefficient (larger than 10{sup 4} mL·g{sup -1}) regardless of the salt concentration. Therefore, the composite adsorbent synthesized in this study is an optimized material considering both the high selectivity of PCFC on Cs and the physical stability of CHA. It is proved that this composite adsorbent can remove rapidly Cs contained in high radioactive/high salt-laden liquid waste with high efficiency.

  9. A novel route to synthesis of glycerol dimethyl ether from epichlorohydrin with high selectivity

    International Nuclear Information System (INIS)

    Ding, Xiaoshu; Liu, Hao; Yang, Qiusheng; Li, Naihua; Dong, Xiangmo; Wang, Shufang; Zhao, Xinqiang; Wang, Yanji

    2014-01-01

    The effective utilization of glycerol, a by-product in the production of biodiesel, into useful chemicals is desirable from the viewpoint of green chemistry. With this in mind, a novel and highly selective route to synthesizing glycerol dimethyl ether (2,3-dimethoxy-1-propanol), a potential fuel additive, from glycerol was proposed. This route uses both glycerol and methanol as starting materials, takes epichlorohydrin as an intermediate product, and utilizes HCl as a recycling agent. Hereinto, the key step of this route is the reaction between epichlorohydrin and methanol to produce 2,3-dimethoxy-1-propanol which is identified by GC–MS, ESI-MS, IR and NMR. The thermodynamics of this reaction was analyzed and the result showed that the thermodynamics of a reaction was favorable and a high product yield was expected. The effect of various parameters such as kind of acid catalyst, molar ratio of epichlorohydrin to methanol, reaction temperature and reaction time was studied. Among various acid catalysts investigated, the acidic ionic liquid [HSO 3 -b-N(CH 3 ) 3 ]HSO 4 exhibited the highest activity and selectivity: conversion of epichlorohydrin of 100% and selectivity of 2,3-dimethoxy-1-propanol of 99% at 393 K, 10 h, an initial pressure of 0.1 MPa and a molar ratio of catalyst:ECH:CH 3 OH of 0.01:1:5. After the reaction, [HSO 3 -b-N(CH 3 ) 3 ]HSO 4 was separated by vacuum distillation and then reused for the next cycle directly. The results showed that the product selectivity remained at about 94% but the conversion of epichlorohydrin dropped to 75% after being used five times. Subsequently, a reaction mechanism for the synthesis of 2,3-dimethoxy-1-propanol from epichlorohydrin and methanol was proposed. - Highlights: • Epichlorohydrin was converted effectively into glycerol dimethyl ether used as potential fuel additive. • The selectivity of 99% and the conversion of 100% under the mild reaction condition. • The reaction was high product selectivity and

  10. Rhodium-catalyzed [5 + 2 + 1] cycloaddition of ene-vinylcyclopropanes and CO: reaction design, development, application in natural product synthesis, and inspiration for developing new reactions for synthesis of eight-membered carbocycles.

    Science.gov (United States)

    Wang, Yi; Yu, Zhi-Xiang

    2015-08-18

    Practical syntheses of natural products and their analogues with eight-membered carbocyclic skeletons are important for medicinal and biological investigations. However, methods and strategies to construct the eight-membered carbocycles are limited. Therefore, developing new methods to synthesize the eight-membered carbocycles is highly desired. In this Account, we describe our development of three rhodium-catalyzed cycloadditions for the construction of the eight-membered carbocycles, which have great potential in addressing the challenges in the synthesis of medium-sized ring systems. The first reaction described in this Account is our computationally designed rhodium-catalyzed two-component [5 + 2 + 1] cycloaddition of ene-vinylcyclopropanes (ene-VCPs) and CO for the diastereoselective construction of bi- and tricyclic cyclooctenones. The design of this reaction is based on the hypothesis that the C(sp(3))-C(sp(3)) reductive elimination of the eight-membered rhodacycle intermediate generated from the rhodium-catalyzed cyclopropane cleavage and alkene insertion, giving Wender's [5 + 2] cycloadduct, is not easy. Under CO atmosphere, CO insertion may occur rapidly, converting the eight-membered rhodacycle into a nine-membered rhodacycle, which then undergoes an easy C(sp(2))-C(sp(3)) reductive elimination process and furnishes the [5 + 2 + 1] product. This hypothesis was supported by our preliminary DFT studies and also served as inspiration for the development of two [7 + 1] cycloadditions: the [7 + 1] cycloaddition of buta-1,3-dienylcyclopropanes (BDCPs) and CO for the construction of cyclooctadienones, and the benzo/[7 + 1] cycloaddition of cyclopropyl-benzocyclobutenes (CP-BCBs) and CO to synthesize the benzocyclooctenones. The efficiency of these rhodium-catalyzed cycloadditions can be revealed by the application in natural product synthesis. Two eight-membered ring-containing natural products, (±)-asterisca-3(15),6-diene and (+)-asteriscanolide, have been

  11. Highly Efficient Method for the Synthesis of Activated Mesoporous Biocarbons with Extremely High Surface Area for High-Pressure CO2 Adsorption.

    Science.gov (United States)

    Singh, Gurwinder; Lakhi, Kripal S; Kim, In Young; Kim, Sungho; Srivastava, Prashant; Naidu, Ravi; Vinu, Ajayan

    2017-09-06

    A simple and efficient way to synthesize activated mesoporous biocarbons (AMBs) with extremely high BET surface area and large pore volume has been achieved for the first time through a simple solid state activation of freely available biomass, Arundo donax, with zinc chloride. The textural parameters of the AMB can easily be controlled by varying the activation temperature. It is demonstrated that the mesoporosity of AMB can be finely tuned with a simple adjustment of the amount of activating agent. AMB with almost 100% mesoporosity can be achieved using the activating agent and the biomass ratio of 5 and carbonization at 500 °C. Under the optimized conditions, AMB with a BET surface area of 3298 m 2 g -1 and a pore volume of 1.9 cm 3 g -1 can be prepared. While being used as an adsorbent for CO 2 capture, AMB registers an impressively high pressure CO 2 adsorption capacity of 30.2 mmol g -1 at 30 bar which is much higher than that of activated carbon (AC), multiwalled carbon nanotubes (MWCNTs), highly ordered mesoporous carbons, and mesoporous carbon nitrides. AMB also shows high stability with excellent regeneration properties under vacuum and temperatures of up to 250 °C. These impressive textural parameters and high CO 2 adsorption capacity of AMB clearly reveal its potential as a promising adsorbent for high-pressure CO 2 capture and storage application. Also, the simple one-step synthesis strategy outlined in this work would provide a pathway to generate a series of novel mesoporous activated biocarbons from different biomasses.

  12. Synthesis of Colloidal Nanocrystal Heterostructures for High-Efficiency Light Emission

    Science.gov (United States)

    Lu, Yifei

    Group II-VI semiconductor nanocrystals, particularly those based on ZnCdS(Se), can be synthesized using well established chemical colloidal processes, and have been a subject of extensive research over the past decade. Their optical properties can be easily tuned through size and composition variations, making them very attractive for many optoelectronic applications including light-emitting diodes (LEDs) and solar cells. Incorporation of diverse internal heterostructures provides an additional means for tuning the optical and electronic properties of conventional ZnCdS(Se) nanocrystals. Extensive bandgap and strain engineering may be applied to the resultant nanocrystal heterostructures to achieve desirable properties and enhanced performance. Despite the high scientific and practical interests of this unique class of nanomaterials, limited efforts have been made to explore their synthesis and potential device applications. This thesis focuses on the synthesis, engineering, characterization, and device demonstration of two types of CdSe-based nanocrystal heterostructures: core/multishell quantum dots (QDs) and QD quantum wells (QDQWs). Their optical properties have been tuned by bandgap and strain engineering to achieve efficient photoluminescence (PL) and electroluminescence (EL).Firstly, yellow light-emitting CdSe QDs with a strain-compensated ZnS/ZnCdS bilayer shell were synthesized using the successive ion layer adsorption and reaction technique and the effects of the shell on the luminescent properties were investigated. The core/shell/shell QDs enjoyed the benefits of excellent exciton confinement by the ZnS intermediate shell and strain compensation by the ZnCdS outer shell, and exhibited 40% stronger PL and a smaller peak redshift upon shell growth compared to conventional CdSe/ZnCdS/ZnS core/shell/shell QDs with an intermediate lattice adaptor. CdSe/ZnS/ZnCdS QD-LEDs had a luminance of 558 cd/m2 at 20 mA/cm 2, 28% higher than that of CdSe/ZnCdS/ZnS QD

  13. Synthesis and morphological examination of high-purity Ca(OH)2 nanoparticles suitable to consolidate porous surfaces

    Science.gov (United States)

    Madrid, Juan Antonio; Lanzón, Marcos

    2017-12-01

    Adequate synthetic methods to obtain pure Ca(OH)2 nanoparticles are scarcely documented in the literature. This paper presents a complete methodology to obtain highly-pure Ca(OH)2 nanoparticles that are appropriate for strengthening heritage materials. The precipitation synthesis was operated in controlled atmosphere to avoid carbonation by atmospheric CO2. A complete purification method was developed to eliminate the sodium chloride generated in the reaction. Several analytical techniques, such as electrical conductivity, pH, ion chromatography, X-ray diffraction (XRD) and thermogravimetric analysis coupled to mass spectrometry (TGA-MS) were used to analyse both the aqueous medium and solid phase. The amount of material obtained in the synthesis (yield) was quantified throughout the purification procedure. The influence of temperature on the nanoparticles' size and stability was studied by transmission electron microscopy (HRTEM) and sedimentation tests (light scattering). It was found that the synthesis yielded high-purity nanoparticles, whose morphological features were greatly affected by the reaction temperature.

  14. Automated synthesis of an {sup 18}F-labelled pyridine-based alkylating agent for high yield oligonucleotide conjugation

    Energy Technology Data Exchange (ETDEWEB)

    Guggenberg, Elisabeth von; Sader, Jayden A.; Wilson, John S.; Shahhosseini, Soraya; Koslowsky, Ingrid; Wuest, Frank [Edmonton PET Centre, Division of Oncologic Imaging, Department of Oncology, Cross Cancer Institute, 11560 University Ave, Edmonton, AB, T6G 1Z2 (Canada); Mercer, John R. [Edmonton PET Centre, Division of Oncologic Imaging, Department of Oncology, Cross Cancer Institute, 11560 University Ave, Edmonton, AB, T6G 1Z2 (Canada)], E-mail: johnmerc@cancerboard.ab.ca

    2009-09-15

    Alkylating agents have been shown to be very promising for the radiolabelling of oligonucleotides with fluorine-18. In this report we describe the fully automated synthesis of 2-bromo-N-[3-(2-[{sup 18}F]fluoropyridin-3-yloxy)propyl]acetamide ([{sup 18}F]FPyBrA) utilizing a modular synthesis unit. Reaction conditions for the coupling of this pyridine-based alkylating agent at the 5' end of a fully phosphorothioated random 20-mer DNA sequence were optimized to achieve very high radiochemical yields (>90%) and a maximum specific activity of 5-6 GBq/{mu}moL. The potential for rapid purification by solid phase extraction without need of chromatographic isolation of the radiolabelled oligonucleotide presents an overall benefit for the application of oligonucleotides in preclinical studies and potential clinical applications.

  15. Controlled soft-template synthesis of ultrathin C@FeS nanosheets with high-Li-storage performance.

    Science.gov (United States)

    Xu, Chen; Zeng, Yi; Rui, Xianhong; Xiao, Ni; Zhu, Jixin; Zhang, Wenyu; Chen, Jing; Liu, Weiling; Tan, Huiteng; Hng, Huey Hoon; Yan, Qingyu

    2012-06-26

    We report a facile approach to prepare carbon-coated troilite FeS (C@FeS) nanosheets via surfactant-assisted solution-based synthesis. 1-Dodecanethiol is used as both the sulfur source and the surfactant, which may form different-shaped micelles to direct the growth of nanostructures. Under appropriate growth conditions, the iron and sulfur atoms react to form thin layers of FeS while the hydrocarbon tails of 1-dodecanethiol separate the thin FeS layers, which turn to carbon after annealing in Ar. Such an approach can be extended to grow C@FeS nanospheres and nanoplates by modifying the synthesis parameters. The C@FeS nanosheets display excellent Li storage properties with high specific capacities and stable charge/discharge cyclability, especially at fast charge/discharge rates.

  16. Prolonged Adaptation to a Low or High Protein Diet Does Not Modulate Basal Muscle Protein Synthesis Rates - A Substudy.

    Directory of Open Access Journals (Sweden)

    Rick Hursel

    Full Text Available Based on controlled 36 h experiments a higher dietary protein intake causes a positive protein balance and a negative fat balance. A positive net protein balance may support fat free mass accrual. However, few data are available on the impact of more prolonged changes in habitual protein intake on whole-body protein metabolism and basal muscle protein synthesis rates.To assess changes in whole-body protein turnover and basal muscle protein synthesis rates following 12 weeks of adaptation to a low versus high dietary protein intake.A randomized parallel study was performed in 40 subjects who followed either a high protein (2.4 g protein/kg/d or low protein (0.4 g protein/kg/d energy-balanced diet (30/35/35% or 5/60/35% energy from protein/carbohydrate/fat for a period of 12 weeks. A subgroup of 7 men and 8 women (body mass index: 22.8±2.3 kg/m2, age: 24.3±4.9 y were selected to evaluate the impact of prolonged adaptation to either a high or low protein intake on whole body protein metabolism and basal muscle protein synthesis rates. After the diet, subjects received continuous infusions with L-[ring-2H5]phenylalanine and L-[ring-2H2]tyrosine in an overnight fasted state, with blood samples and muscle biopsies being collected to assess post-absorptive whole-body protein turnover and muscle protein synthesis rates in vivo in humans.After 12 weeks of intervention, whole-body protein balance in the fasted state was more negative in the high protein treatment when compared with the low protein treatment (-4.1±0.5 vs -2.7±0.6 μmol phenylalanine/kg/h;P<0.001. Whole-body protein breakdown (43.0±4.4 vs 37.8±3.8 μmol phenylalanine/kg/h;P<0.03, synthesis (38.9±4.2 vs 35.1±3.6 μmol phenylalanine/kg/h;P<0.01 and phenylalanine hydroxylation rates (4.1±0.6 vs 2.7±0.6 μmol phenylalanine/kg/h;P<0.001 were significantly higher in the high vs low protein group. Basal muscle protein synthesis rates were maintained on a low vs high protein diet (0.042

  17. Streptococcus mutans Protein Synthesis during Mixed-Species Biofilm Development by High-Throughput Quantitative Proteomics

    Science.gov (United States)

    Klein, Marlise I.; Xiao, Jin; Lu, Bingwen; Delahunty, Claire M.; Yates, John R.; Koo, Hyun

    2012-01-01

    Biofilms formed on tooth surfaces are comprised of mixed microbiota enmeshed in an extracellular matrix. Oral biofilms are constantly exposed to environmental changes, which influence the microbial composition, matrix formation and expression of virulence. Streptococcus mutans and sucrose are key modulators associated with the evolution of virulent-cariogenic biofilms. In this study, we used a high-throughput quantitative proteomics approach to examine how S. mutans produces relevant proteins that facilitate its establishment and optimal survival during mixed-species biofilms development induced by sucrose. Biofilms of S. mutans, alone or mixed with Actinomyces naeslundii and Streptococcus oralis, were initially formed onto saliva-coated hydroxyapatite surface under carbohydrate-limiting condition. Sucrose (1%, w/v) was then introduced to cause environmental changes, and to induce biofilm accumulation. Multidimensional protein identification technology (MudPIT) approach detected up to 60% of proteins encoded by S. mutans within biofilms. Specific proteins associated with exopolysaccharide matrix assembly, metabolic and stress adaptation processes were highly abundant as the biofilm transit from earlier to later developmental stages following sucrose introduction. Our results indicate that S. mutans within a mixed-species biofilm community increases the expression of specific genes associated with glucan synthesis and remodeling (gtfBC, dexA) and glucan-binding (gbpB) during this transition (Pmutans up-regulates specific adaptation mechanisms to cope with acidic environments (F1F0-ATPase system, fatty acid biosynthesis, branched chain amino acids metabolism), and molecular chaperones (GroEL). Interestingly, the protein levels and gene expression are in general augmented when S. mutans form mixed-species biofilms (vs. single-species biofilms) demonstrating fundamental differences in the matrix assembly, survival and biofilm maintenance in the presence of other

  18. Synthesis of TiC/Ni cermets via mechanically activated self-propagating high-temperature synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Dubois, S.; Heian, E.; Karnatak, N.; Beaufort, M.F. [Lab. de Metallurgie Physique, Futuroscope (France); Vrel, D. [Lab. d' Ingenierie des Materiaux et des Hautes Pressions, Villetaneuse (France)

    2003-07-01

    Stoichiometric mixtures of Ti and C were milled in a high-energy vibratory mill for varying times and the results carefully characterized via X-ray diffraction and TEM. Cermets of stoichiometric TiC and 20 w% Ni were combustion synthesized from non-milled and milled reactant powders, resulting in porous solids composed of roughly spherical TiC particles surrounded by a layer of Ni. Time resolved infrared analysis shows that the kinetics of the reaction performed with milled reactant powders are drastically enhanced over non-milled reactants. This result may be attributed to the microstructure and uniformity of the milled reactant mixtures. It is also demonstrated that mechanical milling of Ti and C powders strongly affects the TiC grain size in the products, most likely due to a reduction in TiC crystal growth as a consequence of the increase in the reaction kinetics. (orig.)

  19. Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Na [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); College of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin, 132022 (China); Li, Hong-Wei, E-mail: lihongwei@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); Wu, Yuqing, E-mail: yqwu@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China)

    2017-03-15

    A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

  20. Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

    International Nuclear Information System (INIS)

    Xu, Na; Li, Hong-Wei; Wu, Yuqing

    2017-01-01

    A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

  1. Synthesis and properties of highly branched Jatropha curcas L. oil derivatives

    NARCIS (Netherlands)

    Daniel, Louis; Ardiyanti, Agnes R.; Schuur, Boelo; Manurung, Robert; Broekhuis, Antonius A.; Heeres, Hero J.

    The synthesis and properties of a number of novel branched Jatropha curcas L. oil (JO) derivatives containing vicinal di-ester units in the fatty acid chains are reported. Both the length (acetyl vs. hexanoyl) and the stereochemistry of the vicinal di-ester units (cis vs. trans) were varied. The

  2. Synthesis of highly substituted diphenylacetamides and diphenylsulfonamides by the goldberg coupling reaction

    OpenAIRE

    Raposo, M. Manuela M.; Pereira, Alexandra M. B.; Campos, Ana M. F. Oliveira; Shannon, Patrick V. R.

    2000-01-01

    We report the synthesis and characterisation of multisubstituted diphenylacetamides, diphenylsulfonamides and diphenylamines (and some observations on cyclisation of the last). ICCTI and CRUP (Portugal) and the British Council for financial support Fundação para a Ciência e a Tecnologia (FCT)

  3. Prodigious Effects of Concentration Intensification on Nanoparticle Synthesis: A High-Quality, Scalable Approach

    KAUST Repository

    Williamson, Curtis B.; Nevers, Douglas R.; Hanrath, Tobias; Robinson, Richard D.

    2015-01-01

    -1000-fold increase in Cu2-xS NP production (>200 g) relative to the current field of large-scale (0.1-5 g yields) and laboratory-scale (<0.1 g) efforts. Compared to conventional synthesis methods (hot injection with dilute precursor concentration

  4. Synthesis of manganese stearate for high density polyethylene (HDPE) and its biodegradation

    Science.gov (United States)

    Aras, Neny Rasnyanti M.; Arcana, I. Made

    2015-09-01

    An oxidant additive is one type of additive used for oxo-biodegradable polymers. This additive was prepared by reaction multivalent transition metals and fatty acids to accelerate the degradation process of polymers by providing a thermal treatment or irradiation with light. This study focused on the synthesis of manganese stearate as an additive for application in High Density Polyethylene (HDPE), and the influence of manganese stearate on the characteristics of HDPE including their biodegradability. Manganese stearate was synthesized by the reaction of stearic acid with sodium hydroxide, and sodium stearate formed was reacted with manganese chloride tetrahydrate to form manganese stearate with a melting point of 100-110 °C. Based on the FTIR spectrum showed absorption peak at wave number around 1560 cm-1 which is an asymmetric vibration of CO functional group that binds to the manganese. The films of oxo-biodegradable polymer were prepared by blending HDPE and manganese stearate additives at various concentrations with using the polymer melting method, followed heating at a temperature of 50°C and 70°C for 10 days. The characterizations of the oxo-biodegradable polymers were carried out by analysis the functional groups (FTIR and ATR),thermal properties (TGA), surface properties (SEM), as well as analysis of the biodegradability (the biodegradation test by using activated sludge, % weight loss). Based on COi indicate that the additive of manganese stearate is active in oxidizing polymer by heating treatment. Results of biodegradation by microorganisms from activated sludge showed that the percentage weight loss of polymers increase with the increasing incubation time and the concentration of manganese stearate in HDPE. Biodegradability of HDPE with the addition of manganese stearate and followed by heating at a higher temperature was better observed. The highest percentage weight loss was obtained at the polymer with concentration of 0.2% manganese stearate

  5. Synthesis of manganese stearate for high density polyethylene (HDPE) and its biodegradation

    Energy Technology Data Exchange (ETDEWEB)

    Aras, Neny Rasnyanti M., E-mail: neny.rasnyanti@gmail.com; Arcana, I Made, E-mail: arcana@chem.itb.ac.id [Inorganic and Physical Chemistry Research Division, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jalan Ganesha 10, Bandung 40132 (Indonesia)

    2015-09-30

    An oxidant additive is one type of additive used for oxo-biodegradable polymers. This additive was prepared by reaction multivalent transition metals and fatty acids to accelerate the degradation process of polymers by providing a thermal treatment or irradiation with light. This study focused on the synthesis of manganese stearate as an additive for application in High Density Polyethylene (HDPE), and the influence of manganese stearate on the characteristics of HDPE including their biodegradability. Manganese stearate was synthesized by the reaction of stearic acid with sodium hydroxide, and sodium stearate formed was reacted with manganese chloride tetrahydrate to form manganese stearate with a melting point of 100-110 °C. Based on the FTIR spectrum showed absorption peak at wave number around 1560 cm{sup −1} which is an asymmetric vibration of CO functional group that binds to the manganese. The films of oxo-biodegradable polymer were prepared by blending HDPE and manganese stearate additives at various concentrations with using the polymer melting method, followed heating at a temperature of 50°C and 70°C for 10 days. The characterizations of the oxo-biodegradable polymers were carried out by analysis the functional groups (FTIR and ATR),thermal properties (TGA), surface properties (SEM), as well as analysis of the biodegradability (the biodegradation test by using activated sludge, % weight loss). Based on COi indicate that the additive of manganese stearate is active in oxidizing polymer by heating treatment. Results of biodegradation by microorganisms from activated sludge showed that the percentage weight loss of polymers increase with the increasing incubation time and the concentration of manganese stearate in HDPE. Biodegradability of HDPE with the addition of manganese stearate and followed by heating at a higher temperature was better observed. The highest percentage weight loss was obtained at the polymer with concentration of 0.2% manganese

  6. Thermodynamic efficiency of synthesis, storage and breakdown of the high-energy metabolites by photosynthetic microalgae

    International Nuclear Information System (INIS)

    Sorgüven, Esra; Özilgen, Mustafa

    2013-01-01

    Lipids and carbohydrates are employed in the nature to store internal energy due to the large number of the high energy atomic bonds in their structure. Internal energy stored in the bonds is used to fuel work producing engines or metabolic activity of living organisms. This paper investigates the thermodynamic efficiency of the glucose and lipid synthesis and breakdown by photosynthetic microalgae. Photosynthetic microalgae are able to convert 3.8% of the solar exergy into the chemical exergy of algal lipid. As the microalgae convert the first product of the photosynthesis, i.e. glucose, into lipid, 47–49% of the chemical exergy is lost. If the microalgal cell consumes the photosynthetically produced glucose for its own energy demand, then about 30% of the glucose exergy can be converted into work potential in case of immediate and short-term energy demands. Organism can convert about 22% of the glucose exergy into work potential after a long-term storage. If the algal lipid is harvested for biodiesel production and the produced biodiesel is combusted in a Diesel engine, then about 17% of the exergy of the photosynthetically produced glucose can be converted into useful work. Biodiesel is among the most popular renewable fuels. The lipids are harvested from their storage in the cells to produce biodiesel before following the lipid breakdown path of the cellular metabolism. Our analysis indicates that, extracting the first product of photosynthesis, i.e. glucose or glucose polymers instead of lipids may be more efficient thermodynamically, if new motors capable to extract their bond energy is developed. - Highlights: • Photosynthetic microalgae convert 3.8% of the solar exergy into the chemical exergy of algal lipid. • Converting the first product of the photosynthesis (glucose) into lipid causes 47–49% of exergy loss. • Organism can convert 30% of the glucose exergy into work potential for its own immediate or short-term energy demand. • Organism can

  7. Synthesis of manganese stearate for high density polyethylene (HDPE) and its biodegradation

    International Nuclear Information System (INIS)

    Aras, Neny Rasnyanti M.; Arcana, I Made

    2015-01-01

    An oxidant additive is one type of additive used for oxo-biodegradable polymers. This additive was prepared by reaction multivalent transition metals and fatty acids to accelerate the degradation process of polymers by providing a thermal treatment or irradiation with light. This study focused on the synthesis of manganese stearate as an additive for application in High Density Polyethylene (HDPE), and the influence of manganese stearate on the characteristics of HDPE including their biodegradability. Manganese stearate was synthesized by the reaction of stearic acid with sodium hydroxide, and sodium stearate formed was reacted with manganese chloride tetrahydrate to form manganese stearate with a melting point of 100-110 °C. Based on the FTIR spectrum showed absorption peak at wave number around 1560 cm −1 which is an asymmetric vibration of CO functional group that binds to the manganese. The films of oxo-biodegradable polymer were prepared by blending HDPE and manganese stearate additives at various concentrations with using the polymer melting method, followed heating at a temperature of 50°C and 70°C for 10 days. The characterizations of the oxo-biodegradable polymers were carried out by analysis the functional groups (FTIR and ATR),thermal properties (TGA), surface properties (SEM), as well as analysis of the biodegradability (the biodegradation test by using activated sludge, % weight loss). Based on COi indicate that the additive of manganese stearate is active in oxidizing polymer by heating treatment. Results of biodegradation by microorganisms from activated sludge showed that the percentage weight loss of polymers increase with the increasing incubation time and the concentration of manganese stearate in HDPE. Biodegradability of HDPE with the addition of manganese stearate and followed by heating at a higher temperature was better observed. The highest percentage weight loss was obtained at the polymer with concentration of 0.2% manganese

  8. Surface-Casting Synthesis of Mesoporous Zirconia with a CMK-5-Like Structure and High Surface Area.

    Science.gov (United States)

    Gu, Dong; Schmidt, Wolfgang; Pichler, Christian M; Bongard, Hans-Josef; Spliethoff, Bernd; Asahina, Shunsuke; Cao, Zhengwen; Terasaki, Osamu; Schüth, Ferdi

    2017-09-04

    About 15 years ago, the Ryoo group described the synthesis of CMK-5, a material consisting of a hexagonal arrangement of carbon nanotubes. Extension of the surface casting synthesis to oxide compositions, however, was not possible so far, in spite of many attempts. Here it is demonstrated, that crystalline mesoporous hollow zirconia materials with very high surface areas up to 400 m 2  g -1 , and in selected cases in the form of CMK-5-like, are indeed accessible via such a surface casting process. The key for the successful synthesis is an increased interaction between the silica hard template surface and the zirconia precursor species by using silanol group-rich mesoporous silica as a hard template. The surface areas of the obtained zirconias exceed those of conventionally hard-templated ones by a factor of two to three. The surface casting process seems to be applicable also to other oxide materials. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Photolithographic Synthesis of High-Density DNA and RNA Arrays on Flexible, Transparent, and Easily Subdivided Plastic Substrates.

    Science.gov (United States)

    Holden, Matthew T; Carter, Matthew C D; Wu, Cheng-Hsien; Wolfer, Jamison; Codner, Eric; Sussman, Michael R; Lynn, David M; Smith, Lloyd M

    2015-11-17

    The photolithographic fabrication of high-density DNA and RNA arrays on flexible and transparent plastic substrates is reported. The substrates are thin sheets of poly(ethylene terephthalate) (PET) coated with cross-linked polymer multilayers that present hydroxyl groups suitable for conventional phosphoramidite-based nucleic acid synthesis. We demonstrate that by modifying array synthesis procedures to accommodate the physical and chemical properties of these materials, it is possible to synthesize plastic-backed oligonucleotide arrays with feature sizes as small as 14 μm × 14 μm and feature densities in excess of 125 000/cm(2), similar to specifications attainable using rigid substrates such as glass or glassy carbon. These plastic-backed arrays are tolerant to a wide range of hybridization temperatures, and improved synthetic procedures are described that enable the fabrication of arrays with sequences up to 50 nucleotides in length. These arrays hybridize with S/N ratios comparable to those fabricated on otherwise identical arrays prepared on glass or glassy carbon. This platform supports the enzymatic synthesis of RNA arrays and proof-of-concept experiments are presented showing that the arrays can be readily subdivided into smaller arrays (or "millichips") using common laboratory-scale laser cutting tools. These results expand the utility of oligonucleotide arrays fabricated on plastic substrates and open the door to new applications for these important bioanalytical tools.

  10. Laser-induced incandescence (LII) diagnostic for in situ monitoring of nanoparticle synthesis in a high-pressure arc discharge

    Science.gov (United States)

    Yatom, Shurik; Vekselman, Vladislav; Mitrani, James; Stratton, Brentley; Raitses, Yevgeny; LaboratoryPlasma Nanosynthesis Team

    2016-10-01

    A DC arc discharge is commonly used for synthesis of carbon nanoparticles, including buckyballs, carbon nanotubes, and graphene flakes. In this work we show the first results of nanoparticles monitored during the arc discharge. The graphite electrode is vaporized by high current (60 A) in a buffer Helium gas leading to nanoparticle synthesis in a low temperature plasma. The arc was shown to oscillate, which can possibly influence the nano-synthesis. To visualize the nanoparticles in-situ we employ the LII technique. The nanoparticles with radii >50 nm, emerging from the arc area are heated with a short laser pulse and incandesce. The resulting radiation is captured with an ICCD camera, showing the location of the generated nanoparticles. The images of incandescence are studied together with temporally synchronized fast-framing imaging of C2 emission, to connect the dynamics of arc instabilities, C2 molecules concentration and nanoparticles. The time-resolved incandescence signal is analyzed with combination of ex-situ measurements of the synthesized nanoparticles and LII modeling, to provide the size distribution of produced nanoparticles. This work was supported by US Department of Energy, Office of Science, Basic Energy Sciences, Materials Sciences and Engineering Division.

  11. Bile acid synthesis is increased in Chilean Hispanics with gallstones and in gallstone high-risk Mapuche Indians.

    Science.gov (United States)

    Gälman, Cecilia; Miquel, Juan Francisco; Pérez, Rosa Maria; Einarsson, Curt; Ståhle, Lars; Marshall, Guillermo; Nervi, Flavio; Rudling, Mats

    2004-03-01

    Gallstone disease is an important, costly health-care problem in Western societies. It is still unclear whether hepatic lipid regulatory enzymes play primary or secondary roles in gallstone formation. In this study, the aim was to investigate whether the synthesis of bile acids and cholesterol is increased in gallstone disease and to test whether such a metabolic change, if present, might occur before gallstone formation. A total of 125 Chilean Hispanic women (80 without gallstones and 45 with gallstones) matched for age and body mass index were investigated, along with 40 Chilean Mapuche Indian women (20 without gallstones and 20 with gallstones), a population group in which the prevalence for gallstone disease is very high. Fasting blood plasma samples were assayed for 7 alpha-hydroxy-4-cholesten-3-one and lathosterol, 2 strong indicators for hepatic bile acid and body cholesterol synthesis, respectively. Plasma 7 alpha-hydroxy-4-cholesten-3-one levels, corrected for plasma cholesterol, were significantly increased by 50% in Hispanic women with gallstones as compared with gallstone-free Hispanics (P or =100% (P Mapuche Indian women, independently of whether gallstones were present. Plasma lathosterol, corrected for plasma cholesterol, was significantly increased by 22% in Hispanic women with gallstones and in Mapuche Indian women compared with Hispanic women. The results indicate that the synthesis of bile acids and cholesterol is induced in gallstone disease and precedes gallstone development. These inductions presumably occur as a response to an increased intestinal loss of bile acids.

  12. Methanesulfonic acid-assisted synthesis of N/S co-doped hierarchically porous carbon for high performance supercapacitors

    Science.gov (United States)

    Huo, Silu; Liu, Mingquan; Wu, Linlin; Liu, Mingjie; Xu, Min; Ni, Wei; Yan, Yi-Ming

    2018-05-01

    Nitrogen and sulfur co-doped carbons are considered as electrode materials for high performance supercapacitors, while their further development is still limited by complicated synthesis procedure, unsatisfied structure and low energy density. Developing a simple synthetic strategy to obtain rationally structured carbon materials and high supercapacitor performance is remaining a grand challenge. Herein, we describe the synthesis of nitrogen and sulfur co-doped hierarchical porous carbons as high performance supercapacitors electrode by a methanesulfonic acid-assisted one-step carbonization and activation of the freeze-dried precursors mixture. The as-prepared carbon material not only exhibits ideally hierarchical pores, but also realizes uniform nitrogen and sulfur co-doping. In 6.0 M KOH electrolyte, the material can achieve a high specific capacitance of 272 F g-1 at 1.0 A g-1 and a promising rate performance retaining 172 F g-1 even at 100 A g-1. Moreover, a fabricated symmetric supercapacitor based on as-prepared nitrogen and sulfur co-doped hierarchical porous carbon delivers high energy densities of 12.4 W h kg-1 and 8.0 W h kg-1 in 6.0 M KOH liquid and KOH/PVA solid-state electrolytes, respectively. This work presents a simple and effective methanesulfonic acid-assisted approach for mass production of heteroatomic doping hierarchical porous carbons for future energy storage applications.

  13. Synthesis of chiral N-phosphinyl α-imino esters and their application in asymmetric synthesis of α-amino esters by reduction.

    Science.gov (United States)

    Xiong, Yiwen; Mei, Haibo; Wu, Lingmin; Han, Jianlin; Pan, Yi; Li, Guigen

    2014-01-01

    A variety of chiral N-phosphinyl α-imino esters have been synthesized for the first time from ketoesters and phosphinylamide, which were then reduced by L-selectride to give the corresponding N-phosphinyl-protected α-amino esters. The reduction proceeded very well with excellent chemical yields (88-98%) as well as high diastereoselectivities (96:4 to 99:1). Some of these products could be obtained without column chromatography and recrystallization. The chiral phosphinyl auxiliary could be easily cleaved under acidic conditions.

  14. Synthesis of chiral N-phosphinyl α-imino esters and their application in asymmetric synthesis of α-amino esters by reduction

    Directory of Open Access Journals (Sweden)

    Yiwen Xiong

    2014-03-01

    Full Text Available A variety of chiral N-phosphinyl α-imino esters have been synthesized for the first time from ketoesters and phosphinylamide, which were then reduced by L-selectride to give the corresponding N-phosphinyl-protected α-amino esters. The reduction proceeded very well with excellent chemical yields (88–98% as well as high diastereoselectivities (96:4 to 99:1. Some of these products could be obtained without column chromatography and recrystallization. The chiral phosphinyl auxiliary could be easily cleaved under acidic conditions.

  15. Synthesis of chiral N-phosphinyl α-imino esters and their application in asymmetric synthesis of α-amino esters by reduction

    OpenAIRE

    Xiong, Yiwen; Mei, Haibo; Wu, Lingmin; Han, Jianlin; Pan, Yi; Li, Guigen

    2014-01-01

    A variety of chiral N-phosphinyl α-imino esters have been synthesized for the first time from ketoesters and phosphinylamide, which were then reduced by L-selectride to give the corresponding N-phosphinyl-protected α-amino esters. The reduction proceeded very well with excellent chemical yields (88–98%) as well as high diastereoselectivities (96:4 to 99:1). Some of these products could be obtained without column chromatography and recrystallization. The chiral phosphinyl auxiliary could be ea...

  16. Solid-phase submonomer synthesis of peptoid polymers and their self-assembly into highly-ordered nanosheets.

    Science.gov (United States)

    Tran, Helen; Gael, Sarah L; Connolly, Michael D; Zuckermann, Ronald N

    2011-11-02

    Peptoids are a novel class of biomimetic, non-natural, sequence-specific heteropolymers that resist proteolysis, exhibit potent biological activity, and fold into higher order nanostructures. Structurally similar to peptides, peptoids are poly N-substituted glycines, where the side chains are attached to the nitrogen rather than the alpha-carbon. Their ease of synthesis and structural diversity allows testing of basic design principles to drive de novo design and engineering of new biologically-active and nanostructured materials. Here, a simple manual peptoid synthesis protocol is presented that allows the synthesis of long chain polypeptoids (up to 50mers) in excellent yields. Only basic equipment, simple techniques (e.g. liquid transfer, filtration), and commercially available reagents are required, making peptoids an accessible addition to many researchers' toolkits. The peptoid backbone is grown one monomer at a time via the submonomer method which consists of a two-step monomer addition cycle: acylation and displacement. First, bromoacetic acid activated in situ with N,N'-diisopropylcarbodiimide acylates a resin-bound secondary amine. Second, nucleophilic displacement of the bromide by a primary amine follows to introduce the side chain. The two-step cycle is iterated until the desired chain length is reached. The coupling efficiency of this two-step cycle routinely exceeds 98% and enables the synthesis of peptoids as long as 50 residues. Highly tunable, precise and chemically diverse sequences are achievable with the submonomer method as hundreds of readily available primary amines can be directly incorporated. Peptoids are emerging as a versatile biomimetic material for nanobioscience research because of their synthetic flexibility, robustness, and ordering at the atomic level. The folding of a single-chain, amphiphilic, information-rich polypeptoid into a highly-ordered nanosheet was recently demonstrated. This peptoid is a 36-mer that consists of only

  17. Bromide (Br)--Based Synthesis of Ag Nanocubes with High-Yield.

    Science.gov (United States)

    Wu, Fan; Wang, Wenhui; Xu, Zhongfeng; Li, Fuli

    2015-06-09

    The geometry of metal nanoparticles greatly affects the properties of the localized surface plasmon resonance and surface-enhanced Raman scattering. The synthesis of metal nanoparticles with controllable geometry has thus attracted extensive attentions. In this work, we report a modified polyol synthesis approach of silver (Ag) nanocubes through tuning the concentration of bromide ions (Br(-) ions). We have systematically investigated the effect of Br(-) ions in the polyol process, and find that higher concentration of Br(-) ions can enhance oxidative etching effect, which is the dominative factor in determining nanostructure geometry. Therefore, one can realize control over nanostructure geometry by manipulating the concentration of Br(-) ions. Our work provides an effective approach to control the shape of metallic nanostructures for potential applications.

  18. Bromide (Br) - Based Synthesis of Ag Nanocubes with High-Yield

    Science.gov (United States)

    Wu, Fan; Wang, Wenhui; Xu, Zhongfeng; Li, Fuli

    2015-01-01

    The geometry of metal nanoparticles greatly affects the properties of the localized surface plasmon resonance and surface-enhanced Raman scattering. The synthesis of metal nanoparticles with controllable geometry has thus attracted extensive attentions. In this work, we report a modified polyol synthesis approach of silver (Ag) nanocubes through tuning the concentration of bromide ions (Br− ions). We have systematically investigated the effect of Br− ions in the polyol process, and find that higher concentration of Br− ions can enhance oxidative etching effect, which is the dominative factor in determining nanostructure geometry. Therefore, one can realize control over nanostructure geometry by manipulating the concentration of Br− ions. Our work provides an effective approach to control the shape of metallic nanostructures for potential applications. PMID:26058050

  19. Numerical investigation of high temperature synthesis gas premixed combustion via ANSYS Fluent

    Directory of Open Access Journals (Sweden)

    Pashchenko Dmitry

    2018-01-01

    Full Text Available A numerical model of the synthesis gas pre-mixed combustion is developed. The research was carried out via ANSYS Fluent software. Verification of the numerical results was carried out using experimental data. A visual comparison of the flame contours that obtained by the synthesis gas combustion for Re = 600; 800; 1000 was performed. A comparison of the wall temperature of the combustion chamber, obtained with the help of the developed model, with the results of a physical experiment was also presented. For all cases, good convergence of the results is observed. It is established that a change in the temperature of the syngas/air mixture at the inlet to the combustion chamber does not significantly affect the temperature of the combustion products due to the dissipation of the H2O and CO2 molecules. The obtained results are of practical importance for the design of heat engineering plants with thermochemical heat recovery.

  20. Enzymatic synthesis of bioactive compounds with high potential for cosmeceutical application

    OpenAIRE

    Antonopoulou, Io; Varriale, Simona; Topakas, Evangelos; Rova, Ulrika; Christakopoulos, Paul; Faraco, Vincenza

    2016-01-01

    Cosmeceuticals are cosmetic products containing biologically active ingredients purporting to offer a pharmaceutical therapeutic benefit. The active ingredients can be extracted and purified from natural sources (botanicals, herbal extracts, or animals) but can also be obtained biotechnologically by fermentation and cell cultures or by enzymatic synthesis and modification of natural compounds. A cosmeceutical ingredient should possess an attractive property such as anti-oxidant, anti-inflamma...

  1. A system for the synthesis of uranium hexafluoride by high pressure fluorination of uranium oxides

    International Nuclear Information System (INIS)

    Elizalde T, J.; Saniger B, J.M.; Nava S, R.

    1986-01-01

    An equipment for the synthesis of uranium hexafluoride by a direct fluorination method is reported. The equipment is composed by a gaseous fluorine supply, a gas burette, a reactor tube inside a protective shield, a soda-lime chemical trap and a vacuum system. The fluorination is accomplished at a pressure of about 70 kg/cm 2 (1000 lb in 2 ), using gaseous fluorine. (Author). 5 refs, 4 figs, 2 tabs

  2. Simple, mild, and highly efficient synthesis of 2-substituted benzimidazoles and bis-benzimidazoles

    OpenAIRE

    Eren,Bilge; Bekdemir,Yunus

    2014-01-01

    A new convenient method for preparation of 2-substituted benzimidazoles and bis-benzimidazoles is presented. In this method, o-phenylenediamines were condensed with bisulfite adducts of various aldehydes and di-aldehydes under neat conditions by microwave heating. The results were also compared with results of synthesis by conventional heating under reflux. Structures of the products were confirmed by infrared, ¹H- and 13C-NMR spectroscopy. Short reaction times, good yields, easy purification...

  3. Synthesis of Hafnium-Based Ceramic Materials for Ultra-High Temperature Aerospace Applications

    Science.gov (United States)

    Johnson, Sylvia; Feldman, Jay

    2004-01-01

    This project involved the synthesis of hafnium (Hf)-based ceramic powders and Hf-based precursor solutions that were suitable for preparation of Hf-based ceramics. The Hf-based ceramic materials of interest in this project were hafnium carbide (with nominal composition HE) and hafnium dioxide (HfO2). The materials were prepared at Georgia Institute of Technology and then supplied to research collaborators Dr. Sylvia Johnson and Dr. Jay Feldman) at NASA Ames Research Center.

  4. Highly efficient water-mediated approach to access benzazoles: metal catalyst and base-free synthesis of 2-substituted benzimidazoles, benzoxazoles, and benzothiazoles.

    Science.gov (United States)

    Bala, Manju; Verma, Praveen Kumar; Sharma, Deepika; Kumar, Neeraj; Singh, Bikram

    2015-05-01

    An efficient water-catalyzed method has been developed for the synthesis of 2-substituted benzimidazoles, benzoxazoles, and benzothiazoles in one step. The present method excludes the usage of toxic metal catalysts and bases to produce benzazoles in good to excellent yields. An efficient and versatile water-mediated method has been established for the synthesis of various 2-arylbenzazoles. The present protocol excludes the usage of any catalyst and additive provided excellent selectivities and yields with high functional group tolerance for the synthesis of 2-arylated benzimidazoles, benzoxazoles, and benzothiazoles. Benzazolones were also synthesized using similar reaction protocol.

  5. Seedless Synthesis of Monodispersed Gold Nanorods with Remarkably High Yield: Synergistic Effect of Template Modification and Growth Kinetics Regulation.

    Science.gov (United States)

    Liu, Kang; Bu, Yanru; Zheng, Yuanhui; Jiang, Xuchuan; Yu, Aibing; Wang, Huanting

    2017-03-08

    Gold nanorods (AuNRs) are versatile materials due to their broadly tunable optical properties associated with their anisotropic feature. Conventional seed-mediated synthesis is, however, not only limited by the operational complexity and over-sensitivity towards subtle changes of experimental conditions but also suffers from low yield (≈15 %). A facile seedless method is reported to overcome these challenges. Monodispersed AuNRs with high yield (≈100 %) and highly adjustable longitudinal surface plasmon resonance (LSPR) are reproducibly synthesized. The parameters that influence the AuNRs growth were thoroughly investigated in terms of growth kinetics and soft-template regulation, offering a better understanding of the template-based mechanism. The facile synthesis, broad tunability of LSRP, high reproducibility, high yield, and ease of scale-up make this method promising for the future mass production of monodispersed AuNRs for applications in catalysis, sensing, and biomedicine. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. One-step Synthesis of Pt Nanoparticles Highly Loaded on Graphene Aerogel as Durable Oxygen Reduction Electrocatalyst

    International Nuclear Information System (INIS)

    Huang, Qinghong; Tao, Feifei; Zou, Liangliang; Yuan, Ting; Zou, Zhiqing; Zhang, Haifeng; Zhang, Xiaogang; Yang, Hui

    2015-01-01

    Synthesis of highly active and durable Pt based catalysts with a high metal loading for fuel cells’ applications still remains a big challenge. The three-dimensional (3D) graphene aerogel (GA) not only possess the intrinsic property of graphene, but also have abundant pore architecture for anchoring metal nanoparticles, thus would be suitable as metal catalysts’ support. This work reports a simple and mild one-step co-reduction synthesis of Pt nanoparticles highly loaded on 3D GA and the use as durable oxygen reduction catalyst. Both X-ray diffraction and TEM measurements confirm that Pt nanoparticles (ca. 60 wt.% Pt loading) with an average diameter of ca. 3.2 nm are uniformly decorated on the homogeneously interconnected pores of 3D GA even after a heat treatment at 300 °C. Such a Pt/GA catalyst exhibits significantly enhanced electrocatalytic activity and improved durability for the oxygen reduction reaction. The enhancement in both catalytic activity and durability may result from the unique 3-D architecture structure of GA, the uniform dispersion of Pt nanoparticles, and the interaction between the Pt nanoparticles and GA. The GA-supported Pt can serve as a highly active catalyst for fuel cell applications

  7. DETECTING LOW-LEVEL SYNTHESIS IMPURITIES IN MODIFIED PHOSPHOROTHIOATE OLIGONUCLEOTIDES USING LIQUID CHROMATOGRAPHY – HIGH RESOLUTION MASS SPECTROMETRY

    Science.gov (United States)

    Nikcevic, Irena; Wyrzykiewicz, Tadeusz K.; Limbach, Patrick A.

    2010-01-01

    Summary An LC-MS method based on the use of high resolution Fourier transform ion cyclotron resonance mass spectrometry (FTIRCMS) for profiling oligonucleotides synthesis impurities is described. Oligonucleotide phosphorothioatediesters (phosphorothioate oligonucleotides), in which one of the non-bridging oxygen atoms at each phosphorus center is replaced by a sulfur atom, are now one of the most popular oligonucleotide modifications due to their ease of chemical synthesis and advantageous pharmacokinetic properties. Despite significant progress in the solid-phase oligomerization chemistry used in the manufacturing of these oligonucleotides, multiple classes of low-level impurities always accompany synthetic oligonucleotides. Liquid chromatography-mass spectrometry has emerged as a powerful technique for the identification of these synthesis impurities. However, impurity profiling, where the entire complement of low-level synthetic impurities is identified in a single analysis, is more challenging. Here we present an LC-MS method based the use of high resolution-mass spectrometry, specifically Fourier transform ion cyclotron resonance mass spectrometry (FTIRCMS or FTMS). The optimal LC-FTMS conditions, including the stationary phase and mobile phases for the separation and identification of phosphorothioate oligonucleotides, were found. The characteristics of FTMS enable charge state determination from single m/z values of low-level impurities. Charge state information then enables more accurate modeling of the detected isotopic distribution for identification of the chemical composition of the detected impurity. Using this approach, a number of phosphorothioate impurities can be detected by LC-FTMS including failure sequences carrying 3′-terminal phosphate monoester and 3′-terminal phosphorothioate monoester, incomplete backbone sulfurization and desulfurization products, high molecular weight impurities, and chloral, isobutyryl, and N3 (2-cyanoethyl) adducts

  8. Synthesis of highly stable silver nanoparticles through a novel green method using Mirabillis jalapa for antibacterial, nonlinear optical applications

    Science.gov (United States)

    Pugazhendhi, S.; Palanisamy, P. K.; Jayavel, R.

    2018-05-01

    Green synthesis techniques are developing as more simplistic and eco-friendly approach for the synthesis of metal nanoparticles compared to chemical reduction methods. Herein we report Synthesis of highly stable silver nanoparticles using Mirabillis jalapa seed extract as a reducing and capping agent. The as-prepared silver nanoparticles were characterized by UV-vis spectroscopy (UV-vis) to confirm the formation of silver nanoparticles by its characteristic surface plasmon resonance peak observed at 420 nm. The Powder X-ray diffraction (P-XRD) revealed the structure and crystalline nature of synthesized silver nanoparticles, The Fourier transform infra-red spectroscopic (FT-IR) revealed the presence of the biomolecules in the extract that acted as reducing as well stabilizing agent. The high resolution transmission electron microscopic (HRTEM) images divulged that the synthesized silver nanoparticles were spherical in shape and poly dispersed. The energy dispersive X-ray diffraction (EDX) profile revealed the elements present in the as-synthesized colloidal silver nanoparticles and its percentages. The Zeta potential measured for silver nanoparticles evidenced that the prepared silver nanoparticles owned high stability in room temperature itself. The as-synthesized silver nanoparticles (AgNPs) in colloidal form were showed good antimicrobial effects and it's were found to exhibit third order optical nonlinearity as studied by Z-scan technique using 532 nm Nd:YAG (SHG) CW laser beam (COHERENT-Compass 215 M-50 diode pumped) output as source. The negative nonlinearity observed was well utilized for the study of optical limiting behavior of the silver nanoparticles.

  9. Fluidized bed gasification of high tonnage sorghum, cotton gin trash and beef cattle manure: Evaluation of synthesis gas production

    International Nuclear Information System (INIS)

    Maglinao, Amado L.; Capareda, Sergio C.; Nam, Hyungseok

    2015-01-01

    Highlights: • High tonnage sorghum, cotton gin trash and beef cattle manure were characterized and gasified in a fluidized bed reactor. • Biomass gasification at 730 °C and ER = 0.35 produced synthesis gas with an average energy content of 4.19 MJ Nm −3 . • Synthesis gas heating value and yield were relatively constant at reaction temperatures from 730 °C to 800 °C. • Optimum hydrogen production on HTS gasification was achieved at 780 °C temperature and ER of 0.4. - Abstract: Fluidized bed gasification using high-tonnage sorghum, cotton gin trash and beef cattle manure was performed in a pilot scale bubbling fluidized bed reactor equipped with the necessary feedback control system. Characterization of biomass showed that the high-tonnage sorghum had the highest energy and carbon content of 19.58 MJ kg −1 and 42.29% wt , respectively among the three feed stocks. At 730 °C reaction temperature and equivalence ratio of 0.35, comparable yields of methane, nitrogen and carbon dioxide (within ± 1.4% vol ) were observed in all three feed stocks. The gasification system produced synthesis gas with an average heating value of 4.19 ± 0.09 MJ Nm −3 and an average yield of 1.98 ± 0.1 Nm 3 kg −1 of biomass. Carbon conversion and gasification efficiencies indicated that most of the carbon was converted to gaseous products (85% average ) while 48% average of the energy from the biomass was converted into combustible gas. The production of hydrogen was significantly affected by the biomass used during gasification. The synthesis gas heating value and yield were relatively constant at reaction temperatures from 730 °C to 800 °C. Utilizing high-tonnage sorghum, the optimum hydrogen production during gasification was achieved at a reaction temperature of 780 °C and an equivalence ratio of 0.40.

  10. Highly Atom Economic Synthesis of d?2?Aminobutyric Acid through an In?Vitro Tri?enzymatic Catalytic System

    OpenAIRE

    Chen, Xi; Cui, Yunfeng; Cheng, Xinkuan; Feng, Jinhui; Wu, Qiaqing; Zhu, Dunming

    2017-01-01

    Abstract d?2?Aminobutyric acid is an unnatural amino acid serving as an important intermediate in pharmaceutical production. Developing a synthetic method that uses cheaper starting materials and produces less by?product is a pressing demand. A tri?enzymatic catalytic system, which is composed of l?threonine ammonia lyase (l?TAL), d?amino acid dehydrogenase (d?AADH), and formate dehydrogenase (FDH), has thus been developed for the synthesis of d?2?aminobutyric acid with high optical purity. I...

  11. Synthesis on taking the long term into consideration in the management of high level radioactive wastes. Report nr 293

    International Nuclear Information System (INIS)

    Vaillant, L.; Schneider, T.; Gadbois, S.

    2005-11-01

    The first part of this report proposes a bibliographic synthesis on safety and radiation protection indicators which are used for the assessment of high activity and long-lived waste disposals (conventional indicators, use of radionuclide concentrations or fluxes, and of duration reference), discusses their liability (in relationship with biosphere and meteorology), and discusses their use with respect to the considered time scale. Then, it discusses the expectations of the different stakeholders in Switzerland (the EKRA group), Germany (the AkEnd Committee) and France (stakeholders in Meuse and Haute-Marne)

  12. Synthesis of high specific activity tritium-labelled chloroethylcyclohexylnitrosourea and its application to the study of DNA modification

    Energy Technology Data Exchange (ETDEWEB)

    Siew, E.L. (State Univ. of New York, Albany, NY (USA). Dept. of Chemistry); Habraken, Yvette; Ludlum, D.B. (Massachusetts Univ., Worcester, MA (USA). Medical School)

    1991-02-01

    A small-scale synthesis of high specific activity, N-(2-chloro-2-{sup 3}H-ethyl)-N'-cyclohexyl-N-nitrosourea ({sup 3}H-CCNU) has been accomplished from tritium-labelled ethanolamine. The product is pure by TLC and HPLC analysis and has been used successfully to modify DNA. The overall yield on radioactivity including losses in HPLC purification is approximately 4 percent. The availability of this tritium-labelled compound makes studies of DNA repair and of cellular resistance to N-(2-chloroethyl)-N'-cyclohexyl-N-nitrosourea possible. (author).

  13. Synthesis of high specific activity tritium-labelled chloroethylcyclohexylnitrosourea and its application to the study of DNA modification

    International Nuclear Information System (INIS)

    Siew, E.L.; Habraken, Yvette; Ludlum, D.B.

    1991-01-01

    A small-scale synthesis of high specific activity, N-(2-chloro-2-[ 3 H-ethyl)-N'-cyclohexyl-N-nitrosourea ([ 3 H]-CCNU) has been accomplished from tritium-labelled ethanolamine. The product is pure by TLC and HPLC analysis and has been used successfully to modify DNA. The overall yield on radioactivity including losses in HPLC purification is approximately 4 percent. The availability of this tritium-labelled compound makes studies of DNA repair and of cellular resistance to N-(2-chloroethyl)-N'-cyclohexyl-N-nitrosourea possible. (author)

  14. One-pot synthesis of well-defined polyether/polyester block copolymers and terpolymers by a highly efficient catalyst switch approach

    KAUST Repository

    Alamri, Haleema

    2016-04-20

    A highly efficient methodology, based on a novel catalyst switch approach with rapid crossover characteristics, was developed for the one-pot synthesis of block co/terpolymers of cyclic ethers and esters. This new approach, which takes advantage of one of the best catalysts for epoxide (t-BuP4) and cyclic ester (t-BuP2) polymerization, opens new horizons toward the synthesis of cyclic ether/ester complex macromolecular architectures. © The Royal Society of Chemistry 2016.

  15. One-pot synthesis of well-defined polyether/polyester block copolymers and terpolymers by a highly efficient catalyst switch approach

    KAUST Repository

    Alamri, Haleema; Hadjichristidis, Nikolaos

    2016-01-01

    A highly efficient methodology, based on a novel catalyst switch approach with rapid crossover characteristics, was developed for the one-pot synthesis of block co/terpolymers of cyclic ethers and esters. This new approach, which takes advantage of one of the best catalysts for epoxide (t-BuP4) and cyclic ester (t-BuP2) polymerization, opens new horizons toward the synthesis of cyclic ether/ester complex macromolecular architectures. © The Royal Society of Chemistry 2016.

  16. Facile Synthesis and High performance of a New Carbazole-Based Hole Transporting Material for Hybrid Perovskite Solar Cells

    KAUST Repository

    Wang, Hong

    2015-06-26

    Perovskite solar cells are very promising for practical applications owing to their rapidly rising power conversion efficiency and low cost of solution-based processing. 2,2’,7,7’-tetrakis-(N,N-di-p-methoxyphenylamine) 9,9’-spirobifluorene (Spiro-OMeTAD) is most widely used as hole transporting material (HTM) in perovskite solar cells. However, the tedious synthesis and high cost of Spiro-OMeTAD inhibit its commercial-scale application in the photovoltaic industry. In this article, we report a carbazole-based compound (R01) as a new HTM in efficient perovskite solar cells. R01 is synthesized via a facile route consisting of only two steps from inexpensive commercially available materials. Furthermore, R01 exhibits higher hole mobility and conductivity than the state-of-the-art Spiro-OMeTAD. Perovskite solar cells fabricated with R01 produce a power conversion efficiency of 12.03%, comparable to that obtained in devices using Spiro-OMeTAD in this study. Our findings underscore R01 as a highly promising HTM with high performance, and its facile synthesis and low cost may facilitate the large-scale applications of perovskite solar cells.

  17. Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

    Science.gov (United States)

    Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

    2015-05-01

    The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

  18. Facile Synthesis and High performance of a New Carbazole-Based Hole Transporting Material for Hybrid Perovskite Solar Cells

    KAUST Repository

    Wang, Hong; Sheikh, Arif D.; Feng, Quanyou; Li, Feng; Chen, Yin; Yu, Weili; Alarousu, Erkki; Ma, Chun; Haque, Mohammed; Shi, Dong; Wang, Zhong-Sheng; Mohammed, Omar F.; Bakr, Osman; Wu, Tao

    2015-01-01

    Perovskite solar cells are very promising for practical applications owing to their rapidly rising power conversion efficiency and low cost of solution-based processing. 2,2’,7,7’-tetrakis-(N,N-di-p-methoxyphenylamine) 9,9’-spirobifluorene (Spiro-OMeTAD) is most widely used as hole transporting material (HTM) in perovskite solar cells. However, the tedious synthesis and high cost of Spiro-OMeTAD inhibit its commercial-scale application in the photovoltaic industry. In this article, we report a carbazole-based compound (R01) as a new HTM in efficient perovskite solar cells. R01 is synthesized via a facile route consisting of only two steps from inexpensive commercially available materials. Furthermore, R01 exhibits higher hole mobility and conductivity than the state-of-the-art Spiro-OMeTAD. Perovskite solar cells fabricated with R01 produce a power conversion efficiency of 12.03%, comparable to that obtained in devices using Spiro-OMeTAD in this study. Our findings underscore R01 as a highly promising HTM with high performance, and its facile synthesis and low cost may facilitate the large-scale applications of perovskite solar cells.

  19. Measurement of cross-linked elastin synthesis in bleomycin-induced pulmonary fibrosis using a highly sensitive assay for desmosine and isodesmosine

    International Nuclear Information System (INIS)

    Cantor, J.O.; Osman, M.; Keller, S.; Cerreta, J.M.; Mandl, I.; Turino, G.M.

    1984-01-01

    Cross-linked elastin synthesis was measured in the intratracheal bleomycin model of interstitial pulmonary fibrosis by incorporation of 14C-lysine into the elastin-specific crosslinks, desmosine and isodesmosine. Detection of the labeled crosslinks was facilitated by development of a highly sensitive assay utilizing thin-layer electrophoresis. The results indicate that crosslinked elastin synthesis is significantly elevated from controls (p less than 0.05) at 1 to 3 weeks after exposure to bleomycin and returns to normal by 5 weeks. The increases in labeled elastin synthesis are not directly related to changes in either total lung protein synthesis or the pool size of the 14C-lysine. In comparison with collagen and glycosaminoglycan synthesis in this model of lung injury, maximal increases in cross-linked elastin formation occur later, but overlap with the elevated synthesis of these other connective tissue components. The marked increase from normal in cross-linked elastin synthesis in this model suggests that this tissue component is an important part of the fibrotic response of the pulmonary parenchyma and may play a role in the observed alterations in lung structure and function

  20. High-pressure synthesis of rhombohedral α-AgGaO{sub 2} via direct solid state reaction

    Energy Technology Data Exchange (ETDEWEB)

    Akhtar, Meysam [Department of Physics and Astronomy, University of Louisville, 102 Natural Science Building, Louisville, KY 40292 (United States); Menon, Madhu [Center for Computational Sciences, University of Kentucky, 325 McVey Hall, Lexington, KY 40506 (United States); Sunkara, Mahendra [Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States); Sumanasekera, Gamini [Department of Physics and Astronomy, University of Louisville, 102 Natural Science Building, Louisville, KY 40292 (United States); Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States); Durygin, Andriy [Center for the Study of Matter at Extreme Conditions, Florida International University, VH 140, University Park, Miami, FL 33199 (United States); Jasinski, Jacek B., E-mail: jacek.jasinski@louisville.edu [Conn Center for Renewable Energy Research, University of Louisville, Ernst Hall Room 102A, Louisville, KY 40292 (United States)

    2015-08-25

    Highlights: • Direct synthesis of α-AgGaO{sub 2} via a solid state reaction of Ag{sub 2}O and Ga{sub 2}O{sub 3} powders. • Utilizing high pressure diamond anvil cell to facilitate solid state reaction. • Experimental and theoretical study of vibrational modes for α-AgGaO{sub 2}. • Extensive characterization of synthesized α-AgGaO{sub 2} samples. • GGA + U formalism-based DFT calculations of electronic structure and band gap in α-AgGaO{sub 2}. - Abstract: In this work, we demonstrate the application of high pressure conditions to enable the direct synthesis of α-AgGaO{sub 2} via a solid state reaction of Ag{sub 2}O and Ga{sub 2}O{sub 3}. Synthesis experiments were carried out at pressures and temperatures up to ∼10 GPa and ∼600 °C, respectively, using a resistively-heated diamond anvil cell. Thus synthesized α-AgGaO{sub 2} samples were characterized and their chemical composition and crystal structure were confirmed. In particular, electron diffraction confirmed the rhombohedral delafossite crystal structure of the synthesized AgGaO{sub 2} and its corresponding lattice parameters of a = 2.99 Å and c = 18.43 Å. The vibrational modes analysis was also conducted using a combination of ab initio density functional theory (DFT) and Raman spectroscopy. This analysis yielded good agreement between the calculated Raman-active modes and experimental Raman data. Finally, the application of the GGA + U formalism-based on DFT to calculate the electronic band structure of α-AgGaO{sub 2} provided a more realistic theoretical band gap value than those reported previously.

  1. High yield and facile microwave-assisted synthesis of conductive H_2SO_4 doped polyanilines

    International Nuclear Information System (INIS)

    Gizdavic-Nikolaidis, Marija R.; Jevremovic, Milutin M.; Milenkovic, Maja; Allison, Morgan C.; Stanisavljev, Dragomir R.; Bowmaker, Graham A.; Zujovic, Zoran D.

    2016-01-01

    The microwave-assisted synthesis of polyaniline (PANI) was performed using ammonium persulphate (APS) as oxidizing agent in 0.5 M–2.5 M concentration range of aqueous sulphuric acid (H_2SO_4) at 93 W applied microwave power of 10 min duration. The microwave (MW) synthesized PANIs had 3 times higher yield in comparison to PANI samples prepared using a classical method, CS (0 W MW power) at the same temperature for 10 min synthesis duration period. Fourier Transform Infrared (FTIR) and UV–Vis spectroscopies confirmed the formation of PANI structure in all products. The influence of H_2SO_4 acid dopant on the spin concentration of MW and CS H_2SO_4 doped PANI samples were examined by EPR spectroscopy, while the morphological characteristics were investigated by using scanning electron microscopy (SEM). XRD results showed amorphous phases in both MW and CS H_2SO_4 doped PANI samples. Conductivity measurements revealed ∼1.5 times higher conductivity values for MW H_2SO_4 doped PANI samples in comparison with PANI samples prepared by the CS method under same condition. The influence of sulfate anion in comparison to chloride anion as a dopant on morphological, dopant levels and conductivity properties of MW PANI samples were also investigated. - Highlights: • Nanoporous microwave synthesized doped polyanilines as chemical sensor material. • Morphology and physical properties of polyanilines depend on acid concentration. • Spin concentration is determined by the nature of the polyaniline synthesis.

  2. Long-term rates of mitochondrial protein synthesis are increased in mouse skeletal muscle with high-fat feeding regardless of insulin-sensitizing treatment.

    Science.gov (United States)

    Newsom, Sean A; Miller, Benjamin F; Hamilton, Karyn L; Ehrlicher, Sarah E; Stierwalt, Harrison D; Robinson, Matthew M

    2017-11-01

    Skeletal muscle mitochondrial protein synthesis is regulated in part by insulin. The development of insulin resistance with diet-induced obesity may therefore contribute to impairments to protein synthesis and decreased mitochondrial respiration. Yet the impact of diet-induced obesity and insulin resistance on mitochondrial energetics is controversial, with reports varying from decreases to increases in mitochondrial respiration. We investigated the impact of changes in insulin sensitivity on long-term rates of mitochondrial protein synthesis as a mechanism for changes to mitochondrial respiration in skeletal muscle. Insulin resistance was induced in C57BL/6J mice using 4 wk of a high-fat compared with a low-fat diet. For 8 additional weeks, diets were enriched with pioglitazone to restore insulin sensitivity compared with nonenriched control low-fat or high-fat diets. Skeletal muscle mitochondrial protein synthesis was measured using deuterium oxide labeling during weeks 10-12 High-resolution respirometry was performed using palmitoyl-l-carnitine, glutamate+malate, and glutamate+malate+succinate as substrates for mitochondria isolated from quadriceps. Mitochondrial protein synthesis and palmitoyl- l-carnitine oxidation were increased in mice consuming a high-fat diet, regardless of differences in insulin sensitivity with pioglitazone treatment. There was no effect of diet or pioglitazone treatment on ADP-stimulated respiration or H 2 O 2 emission using glutamate+malate or glutamate+malate+succinate. The results demonstrate no impairments to mitochondrial protein synthesis or respiration following induction of insulin resistance. Instead, mitochondrial protein synthesis was increased with a high-fat diet and may contribute to remodeling of the mitochondria to increase lipid oxidation capacity. Mitochondrial adaptations with a high-fat diet appear driven by nutrient availability, not intrinsic defects that contribute to insulin resistance. Copyright © 2017 the

  3. Simple, mild, and highly efficient synthesis of 2-substituted benzimidazoles and bis-benzimidazoles

    Energy Technology Data Exchange (ETDEWEB)

    Eren, Bilge, E-mail: bilge.eren@bilecik.edu.tr [Faculty of Science and Arts, Department of Chemistry, Bilecik Seyh Edebali University, (Turkey); Bekdemir, Yunus [Faculty of Science and Arts, Canik Basari University, Samsun (Turkey)

    2014-07-01

    A new convenient method for preparation of 2-substituted benzimidazoles and bis-benzimidazoles is presented. In this method, o-phenylenediamines were condensed with bisulfite adducts of various aldehydes and di-aldehydes under neat conditions by microwave heating. The results were also compared with results of synthesis by conventional heating under reflux. Structures of the products were confirmed by infrared, {sup 1}H- and {sup 13}C-NMR spectroscopy. Short reaction times, good yields, easy purification of products, and mild reaction conditions are the main advantages of this method. (author)

  4. Optimization of the synthesis of a high specific activity 125I-labelled hapten for radioimmunoassays

    International Nuclear Information System (INIS)

    Suraez, C.; Paz, D.; Simon, M. A.; Romero del Hombrebueno, B.

    1994-01-01

    In this first report it is described the synthesis, separation and purification of the 2-radioiodinated histamine- I-labelled histamine by a mixed anhydride reaction. About 75% incorporation of I - 125, from Na 1 25I, was achieved with a molecular ratio of 1:1 mixed anhydride:histamine. The radiochemical purity of the conjugate by TLC was > 99% and its theoretical specific activity, 3850 μCi/μg. Dissolved in ethanol and held at -20 degree centigree under darkness decomposition on storage didn't exceed 1% per month. (Author) 13 refs

  5. Optimization of the synthesis of a high specific activity 125 I-labelled hapten for radioimmunoassays

    International Nuclear Information System (INIS)

    Suarez, C.; Simon, M.A.; Paz, D.; Romero del Hombrebueno, B.

    1994-01-01

    In this first report it is described the synthesis, separation and purification of the 2-radioiodinated histamine ''125 I-labelled histamine by a mixed anhydride reaction. About 75% incorporation of I''1125, from Na''125, I, was achieved with a molecular ratio of 1:1 mixed anhydride:histamine. The radiochemical purity of the conjugate by TLC was >99% and its theoretical specific activity, 3850 mu Ci/mug. Dissolved in ethanol and held at -20 degree centigree under darkness decomposition on storage did not exceed 1% per month

  6. Highly efficient and eco-friendly gold-catalyzed synthesis of homoallylic ketones

    KAUST Repository

    Gómez-Suárez, Adrián

    2014-08-01

    We report a new catalytic protocol for the synthesis of γ,δ-unsaturated carbonyl units from simple starting materials, allylic alcohols and alkynes, via a hydroxalkoxylation/Claisen rearrangement sequence. This new process is more efficient (higher TON and TOF) and more eco-friendly (increased mass efficiency) than the previous state-of-the-art technique. In addition, this method tolerates both terminal and internal alkynes. Moreover, computational studies have been carried out in order to shed light on how the Claisen rearrangement is initiated. © 2014 American Chemical Society.

  7. Highly efficient and eco-friendly gold-catalyzed synthesis of homoallylic ketones

    KAUST Repository

    Gó mez-Suá rez, Adriá n; Gasperini, Danila; Vummaleti, Sai V. C.; Poater, Albert; Cavallo, Luigi; Nolan, Steven P.

    2014-01-01

    We report a new catalytic protocol for the synthesis of γ,δ-unsaturated carbonyl units from simple starting materials, allylic alcohols and alkynes, via a hydroxalkoxylation/Claisen rearrangement sequence. This new process is more efficient (higher TON and TOF) and more eco-friendly (increased mass efficiency) than the previous state-of-the-art technique. In addition, this method tolerates both terminal and internal alkynes. Moreover, computational studies have been carried out in order to shed light on how the Claisen rearrangement is initiated. © 2014 American Chemical Society.

  8. High-Quality ZnCdS Nanosheets Prepared Using Solvothermal Synthesis

    International Nuclear Information System (INIS)

    Mahdi, M.A.; Hassan, J.J.; Ng, S.S.; Hassan, Z.

    2013-01-01

    For the first time, Zn X Cd 1-X S nanosheets with different Zn and Cd ion concentrations were prepared using solvothermal synthesis at 200 degree C for 4 and 24 h. The crystalline structure of the nanosheets was wurtzite. The optical band gaps of the nanosheets increased with increasing Zn ratio; this increase is consistent with the band gaps estimated using Vegard’s formula. The photoluminescence spectra for the 24 h nanosheets had higher emission intensities than those for the 4 h nanosheets. The emission band corresponding to intrinsic near-band-edge emission and a broad peak associated with extrinsic deep-level emission were observed in the photoluminescence spectra.

  9. Simple, mild, and highly efficient synthesis of 2-substituted benzimidazoles and bis-benzimidazoles

    International Nuclear Information System (INIS)

    Eren, Bilge; Bekdemir, Yunus

    2014-01-01

    A new convenient method for preparation of 2-substituted benzimidazoles and bis-benzimidazoles is presented. In this method, o-phenylenediamines were condensed with bisulfite adducts of various aldehydes and di-aldehydes under neat conditions by microwave heating. The results were also compared with results of synthesis by conventional heating under reflux. Structures of the products were confirmed by infrared, 1 H- and 13 C-NMR spectroscopy. Short reaction times, good yields, easy purification of products, and mild reaction conditions are the main advantages of this method. (author)

  10. Simple, mild, and highly efficient synthesis of 2-substituted benzimidazoles and bis-benzimidazoles

    Directory of Open Access Journals (Sweden)

    Bilge Eren

    2014-01-01

    Full Text Available A new convenient method for preparation of 2-substituted benzimidazoles and bis-benzimidazoles is presented. In this method, o-phenylenediamines were condensed with bisulfite adducts of various aldehydes and di-aldehydes under neat conditions by microwave heating. The results were also compared with results of synthesis by conventional heating under reflux. Structures of the products were confirmed by infrared, ¹H- and 13C-NMR spectroscopy. Short reaction times, good yields, easy purification of products, and mild reaction conditions are the main advantages of this method.

  11. The synthesis of a high quality, low cost silicon nitride powder by the carbothermal reduction of silica

    International Nuclear Information System (INIS)

    Cochran, G.A.; Conner, C.L.; Eisman, G.A.; Weimer, A.W.; Carroll, D.F.; Dunmead, S.D.; Hwang, C.J.

    1994-01-01

    The development and emergence of silicon nitride in the marketplace depends on the availability of a high quality, low cost powder which meets or exceeds the requirements for the customer's part application. The Dow Chemical Company, funded by the United States Department of Energy Oak Ridge National Laboratory, is engaged in developing a process which will economically synthesize commercial quantities of such a high quality powder. The Dow Chemical Company's approach is based on the carbothermal reduction of silica and has been shown to produce a sub-micron, equi-axed powder with high alpha content (> 95%), low oxygen (< 2%), and minimal carbon and impurities. This paper will review The Dow Chemical Company program and present preliminary results of the synthesis and powder processing efforts. (orig.)

  12. In Situ One-Step Synthesis of Hierarchical Nitrogen-Doped Porous Carbon for High Performance Supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Jeon, Ju Won [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Texas A & M Univ., College Station, TX (United States); Sharma, Ronish [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Meduri, Praveen [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Arey, Bruce W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Schaef, Herbert T. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lutkenhaus, Jodie [Texas A & M Univ., College Station, TX (United States); Lemmon, John P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Thallapally, Praveen K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nandasiri, Manjula I. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); McGrail, B. Peter [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nune, Satish K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2014-04-30

    Electrochemical performance of the existing state-of-the art capacitors is not very high, key scientific barrier is that its charge storage mechanism wholly depends on adsorption of electrolyte on electrode. We present a novel method for the synthesis of nitrogen -doped porous carbons and address the drawback by precisely controlling composition and surface area. Nitrogen-doped porous carbon was synthesized using a self-sacrificial template technique without any additional nitrogen and carbon sources. They exhibited exceptionally high capacitance (239 Fg-1) due to additional pseudocapacitance originating from doped nitrogen. Cycling tests showed no obvious capacitance decay even after 10,000 cycles, which meets the requirement of commercial supercapacitors. Our method is simple and highly efficient for the production of large quantities of nitrogen-doped porous carbons.

  13. Optimization of self-propagating high-temperature synthesis using a halogen fluoride as an igniter for reagents

    Science.gov (United States)

    Gaidar, S. M.; Karelina, M. Yu.; Zhigarev, V. D.

    2016-12-01

    The minimum quantity of the high-activity chemical reagent (HACR) that is required for the initiation of self-propagating high-temperature synthesis (SHS) is determined. The experimental results show that 1-1.3 mg ClF3 (gravity flow from a dosing device), BrF3 on the end of a filling knife, or a few ClF2 + SbF6 - crystals are sufficient for the initiation of titanium-boron or titanium-carbon high-energy powder charge compositions. Since the quantity of HACR required for SHS initiation is very small, the chemical method of initiation can be used for the development of a mobile ignition device for estimating the ignition of various SHS charge compositions under laboratory conditions and for application in standard reactors.

  14. Facile synthesis of uniform MWCNT@Si nanocomposites as high-performance anode materials for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Yifan; Du, Ning, E-mail: dna1122@zju.edu.cn; Zhang, Hui; Yang, Deren

    2015-02-15

    Highlights: • A uniform SiO{sub 2} layer was deposited on multi-walled carbon nanotube. • Synthesis of uniform (MWCNT)@Si nanocomposites via the magnesiothermic reduction. • The MWCNT@Si nanocomposites show high reversible capacity and good cyclability. • Enhanced performance is attributed to porous nanostructure, introduction of MWCNTs. - Abstract: We demonstrate the synthesis of uniform multi-walled carbon nanotube (MWCNT)@Si nanocomposites via the magnesiothermic reduction of pre-synthesized MWCNT@SiO{sub 2} nanocables. At first, the acid vapor steaming is used to treat the surface, which can facilitate the uniform deposition of SiO{sub 2} layer via the TEOS hydrolysis. Then, the uniform MWCNT@Si nanocomposites are obtained on the basis of MWCNT@SiO{sub 2} nanocables via a simple magnesiothermic reduction. When used as an anode material for lithium-ion batteries, the as-synthesized MWCNT@Si nanocomposites show high reversible capacity and good cycling performance, which is better than bulk Si and bare MWCNTs. It is believed that the good electrochemical performance can be attributed to the novel porous nanostructure and the introduction of MWCNTs that can buffer the volume change, maintain the electrical conductive network, and enhance the electronic conductivity and lithium-ion transport.

  15. Synthesis of highly c-oriented ZIF-69 membranes by secondary growth and their gas permeation properties

    KAUST Repository

    Liu, Yunyang; Zeng, Gaofeng; Pan, Yichang; Lai, Zhiping

    2011-01-01

    A seeded growth procedure was successfully developed to synthesize highly c-oriented and well-intergrown zeolitic imidazolate framework-69 (ZIF-69) membranes on porous α-alumina substrates. The synthesis conditions were optimized both for seed preparation and for secondary growth. For seeding, a facile method was developed to prepare smaller and flat ZIF-69 microcrystals in order to make thin and c-oriented seed layers. While for secondary growth, a synthesis condition that favored the growth along the c-direction was chosen in order to form highly c-oriented ZIF-69 membranes after growth. As a result, the majority of ZIF-69 grains inside the membrane have their straight channels along the crystallographic c-axis aligned perpendicularly to the substrate surface. Such alignment was confirmed by both XRD and pole figure analysis. The mixture-gas separation studies that were carried out at room temperature and 1atm gave separation factors of 6.3, 5.0, 4.6 for CO2/N2, CO2/CO and CO2/CH4 respectively, and a permeance of ∼1.0×10-7molm-2s-1Pa-1 for CO2 in almost all mixtures. Both the separation factor and permeance were better than the performance of the ZIF-69 membranes prepared by the in situ solvothermal method due to improvement in the membrane microstructure by the seeded growth method. © 2011 Elsevier B.V.

  16. Phase-controlled synthesis of α-NiS nanoparticles confined in carbon nanorods for High Performance Supercapacitors

    Science.gov (United States)

    Sun, Chencheng; Ma, Mingze; Yang, Jun; Zhang, Yufei; Chen, Peng; Huang, Wei; Dong, Xiaochen

    2014-11-01

    A facile and phase-controlled synthesis of α-NiS nanoparticles (NPs) embedded in carbon nanorods (CRs) is reported by in-situ sulfurating the preformed Ni/CRs. The nanopore confinement by the carbon matrix is essential for the formation of α-NiS and preventing its transition to β-phase, which is in strong contrast to large aggregated β-NiS particles grown freely without the confinement of CRs. When used as electrochemical electrode, the hybrid electrochemical charge storage of the ultrasmall α-NiS nanoparticels dispersed in CRs is benefit for the high capacitor (1092, 946, 835, 740 F g-1 at current densities of 1, 2, 5, 10 A g-1, respectively.). While the high electrochemical stability (approximately 100% retention of specific capacitance after 2000 charge/discharge cycles) is attributed to the supercapacitor-battery electrode, which makes synergistic effect of capacitor (CRs) and battery (NiS NPs) components rather than a merely additive composite. This work not only suggests a general approach for phase-controlled synthesis of nickel sulfide but also opens the door to the rational design and fabrication of novel nickel-based/carbon hybrid supercapacitor-battery electrode materials.

  17. Synthesis of highly c-oriented ZIF-69 membranes by secondary growth and their gas permeation properties

    KAUST Repository

    Liu, Yunyang

    2011-09-01

    A seeded growth procedure was successfully developed to synthesize highly c-oriented and well-intergrown zeolitic imidazolate framework-69 (ZIF-69) membranes on porous α-alumina substrates. The synthesis conditions were optimized both for seed preparation and for secondary growth. For seeding, a facile method was developed to prepare smaller and flat ZIF-69 microcrystals in order to make thin and c-oriented seed layers. While for secondary growth, a synthesis condition that favored the growth along the c-direction was chosen in order to form highly c-oriented ZIF-69 membranes after growth. As a result, the majority of ZIF-69 grains inside the membrane have their straight channels along the crystallographic c-axis aligned perpendicularly to the substrate surface. Such alignment was confirmed by both XRD and pole figure analysis. The mixture-gas separation studies that were carried out at room temperature and 1atm gave separation factors of 6.3, 5.0, 4.6 for CO2/N2, CO2/CO and CO2/CH4 respectively, and a permeance of ∼1.0×10-7molm-2s-1Pa-1 for CO2 in almost all mixtures. Both the separation factor and permeance were better than the performance of the ZIF-69 membranes prepared by the in situ solvothermal method due to improvement in the membrane microstructure by the seeded growth method. © 2011 Elsevier B.V.

  18. ZrC Ceramics Prepared by Self-propagating High-temperature Synthesis/Single Action Pressing

    Directory of Open Access Journals (Sweden)

    CHENG Yong

    2017-01-01

    Full Text Available ZrC ceramics were prepared by mechanical axial compression of self-propagating high-temperature synthesis/single action pressing (SHS/SAP.The effects of pressure on microstructure and densification of the products,as well as the relationship between displacement/variation of the load curve and SHS reaction,were studied.The structure and properties of the products were investigated by XRD and SEM.In addition,the density was measured by the drain away liquid method.Meanwhile,universal testing machine was used to record the displacement and load curve alternations.The results indicate that products are mainly composed of ZrC phase,the process of exhaust are accelerated as the increasing of pressure as well,leading to the smaller size of porosity and crystal particles.Density manifested as an increasing pattern by the elevated pressure with no longer change at 80MPa.Due to the strong attenuation of pressure at the peak of temperature,the density of the production is only 65.7% in 120MPa.The end point of the SHS reaction and the plastic time of the products can be monitored by displacement and load curve.The results provide evidence for the application of self-propagating high-temperature synthesis/pseudo-hot isostatic pressing to further improve the density of ceramics.

  19. Ni foam assisted synthesis of high quality hexagonal boron nitride with large domain size and controllable thickness

    Science.gov (United States)

    Ying, Hao; Li, Xiuting; Li, Deshuai; Huang, Mingqiang; Wan, Wen; Yao, Qian; Chen, Xiangping; Wang, Zhiwei; Wu, Yanqing; Wang, Le; Chen, Shanshan

    2018-04-01

    The scalable synthesis of two-dimensional (2D) hexagonal boron nitride (h-BN) is of great interest for its numerous applications in novel electronic devices. Highly-crystalline h-BN films, with single-crystal sizes up to hundreds of microns, are demonstrated via a novel Ni foam assisted technique reported here for the first time. The nucleation density of h-BN domains can be significantly reduced due to the high boron solubility, as well as the large specific surface area of the Ni foam. The crystalline structure of the h-BN domains is found to be well aligned with, and therefore strongly dependent upon, the underlying Pt lattice orientation. Growth-time dependent experiments confirm the presence of a surface mediated self-limiting growth mechanism for monolayer h-BN on the Pt substrate. However, utilizing remote catalysis from the Ni foam, bilayer h-BN films can be synthesized breaking the self-limiting effect. This work provides further understanding of the mechanisms involved in the growth of h-BN and proposes a facile synthesis technique that may be applied to further applications in which control over the crystal alignment, and the numbers of layers is crucial.

  20. Microwave-Hydrothermal Synthesis and Characterization of High-Purity Nb Doped BaTiO3 Nanocrystals

    Directory of Open Access Journals (Sweden)

    A. Khanfekr

    2014-01-01

    Full Text Available The synthesis of Nb doped BaTiO3 has been investigated under Microwave-Hydrothermal (MH conditions in the temperature of 150°C for only 2 h using C16H36O4Ti, BaH2O2.8H2O and NbCl5 as Ba, Ti and  Nb sources, respectively.  Typical experiments performed on MH processing have not yet reported for Nb doped BaTiO3.  In the MH process, the formation of high purity nano tetragonal Nb-BaTiO3 was strongly enhanced. New hydrothermal method was used instead of the previous solid state reaction for the BaTiO3±Nb2O3 system. The new method uses high pressure to create nano dimension particles in a lower time and temperature. In case of the phase evolution studies, the XRD pattern measurements and Raman spectroscopy were performed. TEM and FE-SEM images were taken for the detailed analysis of the particle size, surface and morphology.  Synthesis of Nb doped BaTiO3 with the Microwave-hydrothermal provides an advantage of fast crystallization and reduced crystal size when compared to existing methods.