Isolation and identification of the thermolabile products of an allene-acetylene-isomerization by high-speed-liquid-chromatography (HSLC)

The thermolabile isomeric acetylenes and allenes were separated from reaction mixtures of the base-catalysed isomerisation of 1,1-diethoxy-hexa-2,5-diyne by preparative HSLC in milligram to gram amounts. This allows a fast and reliable identification by spectroscopic methods. By using fine particle silica (5 μm) for both separations, the analytical one on small columns and the preparative separation on columns with large diameters, the analytical conditions of separation may be transferred to the preparative scale without any difficulty.