Statistical DoE Approach to the Removal of Palladium from Active Pharmaceutical Ingredients (APIs) by Functionalized Silica Adsorbents

The influence of four parameters (temperature, scavenging time, amount of scavenger, and concentration of palladium in the solution) on the efficiency of Pd removal from a cross-coupling reaction, using a commercially available Pd scavenger, SPM32, was studied. The DoE-based method employed yielded...

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Bibliographic Details
Published inOrganic process research & development Vol. 18; no. 5; pp. 626 - 635
Main Authors Recho, Jan, Black, Richard J. G, North, Christopher, Ward, James E, Wilkes, Robin D
Format Journal Article
LanguageEnglish
Published American Chemical Society 16.05.2014
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Summary:The influence of four parameters (temperature, scavenging time, amount of scavenger, and concentration of palladium in the solution) on the efficiency of Pd removal from a cross-coupling reaction, using a commercially available Pd scavenger, SPM32, was studied. The DoE-based method employed yielded more information than is readily attainable from standard adsorption isotherms and kinetics experiments. The optimal regime of scavenging was identified; intuitive and nonintuitive effects of temperature, scavenging time, and scavenger amounts were highlighted; and a mathematical model quantifying predicted Pd removal from the synthetic intermediate was built.
ISSN:1083-6160
1520-586X
DOI:10.1021/op5000336