液体クロマトグラフィーを用いる合成反応生成物の一段階分画単離法

概要

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A simple, one-step fractionation scheme was developed in order to improve currently used isolation techniques for synthetic chemical reactions. Therefore, tedious multi-step processes such as extractions, distillations, and recrystallizations can be excluded. Thin-layer chromatography (TLC) data, used for monitoring and optimizing a synthetic reaction, were directly extrapolated to high performance liquid chromatography (HPLC) system. Inorganic reagents, highly polar side products, and other strongly adsorbed components normally retained at the origin of TLC systems were removed by silica gel pre-column adsorption. Separation of less polar components was performed by HPLC using a solvent system previously selected by TLC examination. The desired products were rapidly fractionated from the crude reaction mixture. General applicability of this method was demonstrated by synthesizing various cholesterol derivatives according to the standard procedure described in Organic Syntheses.
公益社団法人日本薬学会の論文
1977-07-25