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Isolation of pharmaceutical intermediates through solid supported evaporation. batch operation mode / Mebatsion L. Kebede in Industrial & engineering chemistry research, Vol. 51 N° 41 (Octobre 2012) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 51 N° 41 (Octobre 2012) . - pp. 13445–13453 Titre : Isolation of pharmaceutical intermediates through solid supported evaporation. batch operation mode Type de document : texte imprimé Auteurs : Mebatsion L. Kebede, Auteur ; Matthaus U. Babler, Auteur ; Raquel Rozada-Sanchez, Auteur Année de publication : 2012 Article en page(s) : pp. 13445–13453 Note générale : Industrial chemistry Langues : Anglais (eng) Mots-clés : Solid  material  Polymer Résumé : Solid supported evaporation (SSE) is a simple method to isolate dissolved compounds as a solid material. The solution is put in contact with granular porous polymer beads onto which the compounds deposit upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety and handling of the solids. In this paper, SSE in batch mode is explored where the solution is added to the polymer beads at once, i.e. opposite to the semicontinuous mode where the solution is sprayed over a bed of beads. A number of compounds varying widely in their physical and chemical properties is studied. It is found that all compounds could be loaded onto the beads; however, the loading capacity depends on the properties of the compound and in general was lower than in the semicontinuous operating mode studied in an accompanying paper. For highly soluble compounds, higher loadings could be achieved when solvent evaporation was slow. In cases where tested, bead loading was found to be homogeneous within a batch. Recovery of compound from loaded beads was achieved by dispersing the beads in a solvent and washing of the filter cake after filtration. A relatively large amount of solvent is required to achieve full recovery. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie301358x [article] Isolation of pharmaceutical intermediates through solid supported evaporation. batch operation mode [texte imprimé] / Mebatsion L. Kebede, Auteur ; Matthaus U. Babler, Auteur ; Raquel Rozada-Sanchez, Auteur . - 2012 . - pp. 13445–13453. Industrial chemistry Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 51 N° 41 (Octobre 2012) . - pp. 13445–13453 Mots-clés : Solid  material  Polymer Résumé : Solid supported evaporation (SSE) is a simple method to isolate dissolved compounds as a solid material. The solution is put in contact with granular porous polymer beads onto which the compounds deposit upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety and handling of the solids. In this paper, SSE in batch mode is explored where the solution is added to the polymer beads at once, i.e. opposite to the semicontinuous mode where the solution is sprayed over a bed of beads. A number of compounds varying widely in their physical and chemical properties is studied. It is found that all compounds could be loaded onto the beads; however, the loading capacity depends on the properties of the compound and in general was lower than in the semicontinuous operating mode studied in an accompanying paper. For highly soluble compounds, higher loadings could be achieved when solvent evaporation was slow. In cases where tested, bead loading was found to be homogeneous within a batch. Recovery of compound from loaded beads was achieved by dispersing the beads in a solvent and washing of the filter cake after filtration. A relatively large amount of solvent is required to achieve full recovery. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie301358x

Isolation of pharmaceutical intermediates through solid supported evaporation. semicontinuous Operation Mode / Matthaus U. Babler in Industrial & engineering chemistry research, Vol. 51 N° 45 (Novembre 2012) 

Public ISBD [article]  in Industrial & engineering chemistry research > Vol. 51 N° 45 (Novembre 2012) . - pp. 14814–14823 Titre : Isolation of pharmaceutical intermediates through solid supported evaporation. semicontinuous Operation Mode Type de document : texte imprimé Auteurs : Matthaus U. Babler, Auteur ; Mebatsion L. Kebede, Auteur ; Raquel Rozada-Sanchez, Auteur Année de publication : 2013 Article en page(s) : pp. 14814–14823 Note générale : Industrial chemistry Langues : Anglais (eng) Mots-clés : Solid  evaporationi  Solating  nonvolatile Résumé : Solid supported evaporation (SSE) is a simple, nonselective method for isolating nonvolatile compounds from a solution. The solution is put in contact with porous polymer beads onto which the compound deposits upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety, thermal decomposition, and solid handling, as the loaded beads form a free-flowing granular material that is easily recovered. In this paper, SSE in a semicontinuous operating mode is investigated where the solution is continuously fed to (respectively sprayed over) an agitated bed of dry beads put under vacuum. It is found that under conditions where the solvent evaporation rate is high with respect to the feed rate, high bead loadings can be achieved before extensive sticking of beads and compound to the vessel walls occurs. The type of compound and solvent had little influence on the process performance, and, in cases where this was explored, the bead loading was found to be homogeneous. Based on a balance equation for the solvent fed to the system, a model is developed that results in a simple scale up criterion. The latter was successfully applied for transferring SSE from lab to the kilo lab scale. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie301359c [article] Isolation of pharmaceutical intermediates through solid supported evaporation. semicontinuous Operation Mode [texte imprimé] / Matthaus U. Babler, Auteur ; Mebatsion L. Kebede, Auteur ; Raquel Rozada-Sanchez, Auteur . - 2013 . - pp. 14814–14823. Industrial chemistry Langues : Anglais (eng) in Industrial & engineering chemistry research > Vol. 51 N° 45 (Novembre 2012) . - pp. 14814–14823 Mots-clés : Solid  evaporationi  Solating  nonvolatile Résumé : Solid supported evaporation (SSE) is a simple, nonselective method for isolating nonvolatile compounds from a solution. The solution is put in contact with porous polymer beads onto which the compound deposits upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety, thermal decomposition, and solid handling, as the loaded beads form a free-flowing granular material that is easily recovered. In this paper, SSE in a semicontinuous operating mode is investigated where the solution is continuously fed to (respectively sprayed over) an agitated bed of dry beads put under vacuum. It is found that under conditions where the solvent evaporation rate is high with respect to the feed rate, high bead loadings can be achieved before extensive sticking of beads and compound to the vessel walls occurs. The type of compound and solvent had little influence on the process performance, and, in cases where this was explored, the bead loading was found to be homogeneous. Based on a balance equation for the solvent fed to the system, a model is developed that results in a simple scale up criterion. The latter was successfully applied for transferring SSE from lab to the kilo lab scale. ISSN : 0888-5885 En ligne : http://pubs.acs.org/doi/abs/10.1021/ie301359c