A Direct Fractionation Procedure for the Isolation of Synthetic Products Utilizing Normal and Reversed Phase Liquid Chromatography

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Abstract
A simple, one-step fractionation scheme was developed by utilizing liquid chromatography in order to provide new and improved isolation techniques for synthetic reactions, allowing elimination of tedious, multi-step processes presently in use. Thin-layer chromatography (TLC) data, used for monitoring and optimizing synthetic reactions, were directly extrapolated to high performance liquid chromatography (HPLC) systems. Inorganic reagents and highly polar side products were removed by a silica pre-column. A reversed phase column was used for clean-up process. The desired products were rapidly fractionated from the crude reaction mixture. General applicability of this procedure was demonstrated in the syntheses of various steroid derivatives.