Abstract

A range of diastereomeric alkynepentacarbonyldicobalt complexes containing the ( R)-(+)-Glyphos ligand have been prepared in moderate to good yields under standard thermal conditions. Additionally, novel tertiary amine N-oxide mediated reactions have been developed which allow the synthesis of the same range of complexes at room temperature with good selectivity in consistently high yields. Optically pure ( R)-(+)-Glyphos containing complexes have been obtained by preparative HPLC separation of the sets of diastereomeric compounds. Finally, the amine N-oxide techniques allow the rapid and clean preparation of alkynepentacarbonyltriphenylphosphinedicobalt complexes in good to high yields at room temperature.

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