The use of high performance liquid chromatography for the analysis and monitoring of iron carbonyl complexes in a reaction mixture

The suitability of high performance liquid chromatography (HPLC) as an analytical and preparative tool for the analysis and isolation of the products resulting from a reaction of diironnonacarbonyl Fe₂(CO)₉] with di-t-butyl-sulfurdiimine DBSD] was investigated. Reserved phase chromatography with octyl-modified silica as stationary phase and methanol/water mixtures as mobile phase showed a high selectivity for the separation of the products, and by use of gradient elution the separation of 17 products was completed within 30 min, which meant that the progress of the reaction could be monitored, A semi-preparative column (dimensions 250 X 10 mm) was useful in isolating some of the products; with this column 7 mg of reaction products could be injected without loss in efficiency.