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

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• 作者：Christopher J. Welch ; Derek W. Henderson ; Brenda Pipik ; Mohamed Shaimi ; David Schenk ; Dave Conlon
• 刊名：Organic Process Research & Development
• 出版年：2010
• 出版时间：July 16, 2010
• 年：2010
• 卷：14
• 期：4
• 页码：905-907
• 全文大小：117K
• 年卷期：v.14,no.4(July 16, 2010)
• ISSN：1520-586X

文摘

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.