Shortcut to Selectivity: Make Them All and Let Preparative Chromatography Sort it Out

Autor: Derek W. Henderson, Christopher J. Welch, Dave Conlon, Mohamed Shaimi, Brenda Pipik, David J. Schenk
Rok vydání: 2010
Předmět:
Zdroj: Organic Process Research & Development. 14:905-907
ISSN: 1520-586X
1083-6160
DOI: 10.1021/op100095e
Popis: Preparative chromatography was used to overcome the difficult selectivity challenge of accessing a single isomer of a mono tert-butyldimethylsilyl (TBDMS) derivative of an unsymmetrical diol. Chromatographic purification allowed rapid purification of more than 10 kg of the desired intermediate from the statistical mixture of undesired mono-TBDMS, bis-TBDMS, and very strongly retained, unreacted starting material. A noteworthy injection cycle strategy of performing three injections, then desorbing the accumulated strongly bound diol starting material with a strong solvent wash was employed in the separation.
Databáze: OpenAIRE