Preparation and chromatographic separation of diastereoisomeric diaza-diphospha-macrocycles

Chiral macrocyclic binaphthyl derivatives, containing phosphorus and nitrogen hetero atoms, have been prepared as mixtures of three diastereoisomers. Their separation on a preparative scale was achieved after two chromatographic steps using polystyrene gel and strongly deactivated silica gel to avoid irreversible adsorption. A configurational assignment of the diastereoisomers was partly possible on the basis of NMR spectroscopy.