Bulk Mixing in a Milligram-Scale Solid Phase Batch Reactor
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| Titel: | Bulk Mixing in a Milligram-Scale Solid Phase Batch Reactor |
|---|---|
| Autoren: | Sebastián Pinzón-López, Dominik Ebert, Emelie E. Reuber, Matthias Kraume, Peter H. Seeberger, José Danglad-Flores |
| Quelle: | Organic Process Research & Development. 29:2275-2286 |
| Verlagsinformationen: | American Chemical Society (ACS), 2025. |
| Publikationsjahr: | 2025 |
| Schlagwörter: | mixing time, bubbling reactor, Mixing, Chemie und zugeordnete Wissenschaften, solid phase synthesis |
| Beschreibung: | Adequate mixing is essential during reactions, especially in heterogeneous systems such as Solid Phase Synthesis (SPS), where the reagents transit from the fluid phase into the solid support. Despite the importance of mixing, a quantitative analysis within a theoretical framework is missing for SPS reactors. We analyze mechanical stirring (100–1300 rpm) and argon bubbling (1–30 cm 3 /min; 0.02–0.70 cm/s) as mixing methods in a milligram-scale batch reactor. Digital Image Analysis (DIA) was used to characterize the liquid mixing and particle dispersion. Typical solvents for SPS of biomoleculesacetonitrile (ACN), dichloromethane (DCM), and dimethylformamide (DMF)were studied. The dispersion model represented the mixing process. Both mixing methods homogenize the liquid in times as short as 1s. Particle dispersion is accomplished in DCM and DMF but is limited in ACN, where the Archimedes number (Ar) was larger. The synthesis of various glycan probes through Automated Glycan Assembly (AGA) suggests that adequate mixing and thermal conditions are indispensable for process optimization. |
| Publikationsart: | Article Other literature type |
| Sprache: | English |
| ISSN: | 1520-586X 1083-6160 |
| DOI: | 10.1021/acs.oprd.5c00194 |
| DOI: | 10.17169/refubium-49218 |
| Rights: | CC BY |
| Dokumentencode: | edsair.doi.dedup.....ba1472888df7baaa3910f34bee7278da |
| Datenbank: | OpenAIRE |
Nájsť tento článok vo Web of Science | Abstract: | Adequate mixing is essential during reactions, especially in heterogeneous systems such as Solid Phase Synthesis (SPS), where the reagents transit from the fluid phase into the solid support. Despite the importance of mixing, a quantitative analysis within a theoretical framework is missing for SPS reactors. We analyze mechanical stirring (100–1300 rpm) and argon bubbling (1–30 cm 3 /min; 0.02–0.70 cm/s) as mixing methods in a milligram-scale batch reactor. Digital Image Analysis (DIA) was used to characterize the liquid mixing and particle dispersion. Typical solvents for SPS of biomoleculesacetonitrile (ACN), dichloromethane (DCM), and dimethylformamide (DMF)were studied. The dispersion model represented the mixing process. Both mixing methods homogenize the liquid in times as short as 1s. Particle dispersion is accomplished in DCM and DMF but is limited in ACN, where the Archimedes number (Ar) was larger. The synthesis of various glycan probes through Automated Glycan Assembly (AGA) suggests that adequate mixing and thermal conditions are indispensable for process optimization. |
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| ISSN: | 1520586X 10836160 |
| DOI: | 10.1021/acs.oprd.5c00194 |