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More benign synthesis of palladium nanoparticles in dimethyl sulfoxide and their extraction into an organic pohase / Juncheng Liu in Industrial & engineering chemistry research, Vol. 49 N° 17 (Septembre 1, 2010) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 49 N° 17 (Septembre 1, 2010) . - pp 8174–8179 Titre : More benign synthesis of palladium nanoparticles in dimethyl sulfoxide and their extraction into an organic pohase Type de document : texte imprimé Auteurs : Juncheng Liu, Auteur ; Nicholas Ruffini, Auteur ; Pamela Pollet, Auteur Année de publication : 2010 Article en page(s) : pp 8174–8179 Note générale : Chimie industrielle Langues : Anglais (eng) Mots-clés : Nanoparticles  Dimethyl  Organic  phase. Résumé : We present the successful synthesis and stabilization of 3.5 nm Pd nanoparticles (standard deviation of 0.49 nm) within dimethyl sulfoxide (DMSO) via fast, homogeneous reduction of a Pd salt using NaBH4 in the absence of traditional capping ligands. These Pd nanoparticles were found to be extremely stable and did not exhibit precipitation and/or agglomeration within the DMSO solvent even after more than 9 months. Moreover, these Pd nanoparticles were conveniently separated from the DMSO solvent medium via vacuum freeze drying by taking advantage of the high freezing point of DMSO. We have also successfully extracted the Pd nanoparticles from the DMSO phase into an organic phase (i.e., hexane), thereby providing a facile and efficient means for the generation of organic phase dispersible metal nanoparticles with complete recycle of the DMSO solvent. DEWEY : 660 ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie902013g [article] More benign synthesis of palladium nanoparticles in dimethyl sulfoxide and their extraction into an organic pohase [texte imprimé] / Juncheng Liu, Auteur ; Nicholas Ruffini, Auteur ; Pamela Pollet, Auteur . - 2010 . - pp 8174–8179. Chimie industrielle Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 49 N° 17 (Septembre 1, 2010) . - pp 8174–8179 Mots-clés : Nanoparticles  Dimethyl  Organic  phase. Résumé : We present the successful synthesis and stabilization of 3.5 nm Pd nanoparticles (standard deviation of 0.49 nm) within dimethyl sulfoxide (DMSO) via fast, homogeneous reduction of a Pd salt using NaBH4 in the absence of traditional capping ligands. These Pd nanoparticles were found to be extremely stable and did not exhibit precipitation and/or agglomeration within the DMSO solvent even after more than 9 months. Moreover, these Pd nanoparticles were conveniently separated from the DMSO solvent medium via vacuum freeze drying by taking advantage of the high freezing point of DMSO. We have also successfully extracted the Pd nanoparticles from the DMSO phase into an organic phase (i.e., hexane), thereby providing a facile and efficient means for the generation of organic phase dispersible metal nanoparticles with complete recycle of the DMSO solvent. DEWEY : 660 ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie902013g

Production of (S)-1-benzyl-3-diazo-2-oxopropylcarbamic acid tert-butyl ester, a diazoketone pharmaceutical intermediate, employing a small scale continuous reactor / Pamela Pollet in Industrial & engineering chemistry research, Vol. 48 N° 15 (Août 2009) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 48 N° 15 (Août 2009) . - pp. 7032–7036 Titre : Production of (S)-1-benzyl-3-diazo-2-oxopropylcarbamic acid tert-butyl ester, a diazoketone pharmaceutical intermediate, employing a small scale continuous reactor Type de document : texte imprimé Auteurs : Pamela Pollet, Auteur ; Elizabeth D. Cope, Auteur ; Michelle K. Kassner, Auteur Année de publication : 2009 Article en page(s) : pp. 7032–7036 Note générale : Chemical engineering Langues : Anglais (eng) Mots-clés : N-Boc-(1S)-benzylhydroxy-3-chloropropylamine  Small  scale  continuous  reactor Résumé : N-Boc-(1S)-benzylhydroxy-3-chloropropylamine (6) is a precursor to pharmaceutically active compounds that act as human immunodeficiency virus (HIV) protease inhibitors. It is currently being produced via a batch process which includes a homologation step with diazomethane. This article considers the challenges faced when converting a traditional batch process to a continuous flow system for the production of the key intermediate (S)-1-benzyl-3-diazo-2-oxopropylcarbamic acid tert-butyl ester (4). A continuous flow reactor was designed, built, and used to carry out a two step reaction sequence: the formation of a temperature sensitive mixed anhydride intermediate (3) and the subsequent reaction of that intermediate (3) with trimethylsilyldiazomethane (8) to yield the diazoketone intermediate (4). By modifying the chemistry and maximizing the mixing and heat transfer, the batch process was successfully converted to a continuous flow process. En ligne : http://pubs.acs.org/doi/abs/10.1021/ie801885y [article] Production of (S)-1-benzyl-3-diazo-2-oxopropylcarbamic acid tert-butyl ester, a diazoketone pharmaceutical intermediate, employing a small scale continuous reactor [texte imprimé] / Pamela Pollet, Auteur ; Elizabeth D. Cope, Auteur ; Michelle K. Kassner, Auteur . - 2009 . - pp. 7032–7036. Chemical engineering Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 48 N° 15 (Août 2009) . - pp. 7032–7036 Mots-clés : N-Boc-(1S)-benzylhydroxy-3-chloropropylamine  Small  scale  continuous  reactor Résumé : N-Boc-(1S)-benzylhydroxy-3-chloropropylamine (6) is a precursor to pharmaceutically active compounds that act as human immunodeficiency virus (HIV) protease inhibitors. It is currently being produced via a batch process which includes a homologation step with diazomethane. This article considers the challenges faced when converting a traditional batch process to a continuous flow system for the production of the key intermediate (S)-1-benzyl-3-diazo-2-oxopropylcarbamic acid tert-butyl ester (4). A continuous flow reactor was designed, built, and used to carry out a two step reaction sequence: the formation of a temperature sensitive mixed anhydride intermediate (3) and the subsequent reaction of that intermediate (3) with trimethylsilyldiazomethane (8) to yield the diazoketone intermediate (4). By modifying the chemistry and maximizing the mixing and heat transfer, the batch process was successfully converted to a continuous flow process. En ligne : http://pubs.acs.org/doi/abs/10.1021/ie801885y