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Recycling Experiments (recycling + experiment)
Selected AbstractsNew route to synthesis of PVP-stabilized palladium(0) nanoclusters and their enhanced catalytic activity in Heck and Suzuki cross-coupling reactionsAPPLIED ORGANOMETALLIC CHEMISTRY, Issue 12 2009Feyyaz Durap Abstract Herein we report a new method for the synthesis and characterization of PVP-stabilized palladium(0) nanoclusters and their enhanced catalytic activity in Suzuki coupling and Heck reactions of aryl bromides with phenylboronic acid and styrene, respectively, under mild conditions. The PVP-stabilized palladium(0) nanoclusters with a particle size of 4.5 ± 1.1 nm were prepared using a new method: refluxing a mixture of potassium tetrachloropalladate(II) and PVP in methanol at 80 °C for 1 h followed by reduction with sodium borohydride. Palladium(0) nanoclusters prepared in this way were stable in solution for weeks, could be isolated as solid materials and were characterized by TEM, XPS, UV,vis, and XRD techniques. The PVP-stabilized palladium(0) nanoclusters were active catalysts in Heck and Suzuki coupling reactions of arylbromides with styrene and phenylboronic acid affording stilbenes and biphenyls, respectively, in high yield. Recycling experiments showed that PVP-stabilized palladium(0) nanoclusters could be used five times with essentially no loss in activity in the Heck and Suzuki coupling reactions. Copyright © 2009 John Wiley & Sons, Ltd. [source] Preparation of 2-Quinolones by Sequential Heck Reduction,Cyclization (HRC) Reactions by Using a Multitask Palladium CatalystCHEMISTRY - A EUROPEAN JOURNAL, Issue 29 2009François-Xavier Felpin Dr. Abstract One-pot sequential Heck reduction,cyclization (HRC) reactions leading to the synthesis of substituted 2-quinolones have been developed by using a heterogeneous or mixed homogeneous/heterogeneous multitask palladium catalyst with charcoal as a support. The whole sequence occurs under very mild conditions without the need for additives (ligand or base) by taking advantage of the high reactivity of aryldiazonium salts as "super electrophiles". Recycling experiments showed that the reused heterogeneous Pd0/C catalyst was not able to promote another HRC sequence but was, however, still highly active for hydrogenation, hydrodehalogenation, as well as hydrogenolysis reactions. [source] Synthesis of Chiral 2-Phospha[3]ferrocenophanes and their Behaviour as Organocatalysts in [3+2],Cyclization ReactionsADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 11-12 2009Arnaud Voituriez Abstract Planar chiral 2-phospha[3]ferrocenophanes have been prepared via a stereoselective three-step synthesis. The key step is the lithiation of the 1,1,-disubstituted ferrocene 11 bearing (S)-2-(methoxymethyl)pyrrolidines as the chiral ortho -directing groups. The diastereoselectivity of these reactions has been mastered by an appropriate choice of the metallating agent, so as to afford a suitable access to C2 -symmetrical, tetrasubstituted ferrocenes. These compounds have been converted into the enantiomerically pure 2-phospha[3]-ferrocenophanes 16, via the corresponding acetates and their reactions with primary phosphines. Phosphines 16 have been used as nucleophilic catalysts in model cyclization reactions. Unlike 2-phospha[3]-ferrocenophanes with stereogenic ,-carbons, the planar chiral derivatives 16 proved to be suitable catalysts for these processes. Thus, for instance, phosphine 16c successfully promotes the enantioselective [3+2],annulations of allenes and enones into functionalized cyclopentenes (ees up to 96%). Among others, spirocyclic derivatives have been obtained in good yields and ees in the range 77,85%. The robustness of this catalyst has been demonstrated by recycling experiments. [source] ,Click' Dendritic Phosphines: Design, Synthesis, Application in Suzuki Coupling, and Recycling by NanofiltrationADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 3 2009Michèle Janssen Abstract A new synthetic route towards stable molecular-weight enlarged monodentate phosphine ligands via ,click' chemistry was developed. These ligands were applied in the Pd-catalyzed Suzuki,Miyaura coupling of aryl halides and phenyl boronic acid. The supported systems show very similar activities compared to the unsupported analogues. Moreover, recycling experiments by means of nanofiltration using ceramic nanofiltration membranes demonstrate that these systems can be recovered and reused efficiently. [source] Simple enzymatic procedure for l -carnosine synthesis: whole-cell biocatalysis and efficient biocatalyst recyclingMICROBIAL BIOTECHNOLOGY, Issue 1 2010Jan Heyland Summary , -Peptides and their derivates are usually stable to proteolysis and have an increased half-life compared with , -peptides. Recently, , -aminopeptidases were described as a new enzyme class that enabled the enzymatic degradation and formation of , -peptides. As an alternative to the existing chemical synthesis routes, the aim of the present work was to develop a whole-cell biocatalyst for the synthesis and production of , -peptides using this enzymatic activity. For the optimization of the reaction system we chose the commercially relevant ,,, -dipeptide l -carnosine (, -alanine- l -histidine) as model product. We were able to show that different recombinant yeast and bacteria strains, which overexpress a , -peptidase, could be used directly as whole-cell biocatalysts for the synthesis of l -carnosine. By optimizing relevant reaction conditions for the best-performing recombinant Escherichia coli strain, such as pH and substrate concentrations, we obtained high l -carnosine yields of up to 71%. Long-time as well as biocatalyst recycling experiments indicated a high stability of the developed biocatalyst for at least five repeated batches. Application of the recombinant E. coli in a fed-batch process enabled the accumulation of l -carnosine to a concentration of 3.7 g l,1. [source] Homogeneous Stabilization of Pt Nanoparticles in Dendritic Core,Multishell Architectures: Application in Catalytic Hydrogenation Reactions and RecyclingCHEMCATCHEM, Issue 7 2010Juliane Keilitz Abstract Core,multishell architectures are a new approach to homogeneously stabilize metal nanoparticles for harsh conditions. Herein, we present the synthesis and stabilization of Pt nanoparticles in dendritic core,multishell polymers and their application in hydrogenation reactions. The successful recycling of the catalyst was demonstrated for the hydrogenation of methyl crotonate 1 and was either achieved by ultrafiltration or in a two-phase system for at least 14,cycles. Thereby, the total turnover number (TON) was increased to 22,000. In the recycling experiments, low metal leaching into the product (as low as 0.3,ppm) was detected. Additionally, the selective hydrogenation of isophorone 3 was investigated and selectivities of 99:1 for CC versus CO hydrogenation were achieved. [source] | ||||||||||