Abstract

A convenient procedure for the synthesis of the rhenium carbonyls Re-2(CO)(10) and Re(CO)(5)Cl is reported. Sodium reduction of the easily available K2ReCl6, under CO presssure (2400 psi, 280 degrees C (external temperature), THF as solvent) affords Re,(CO),, and Re(CO)(5)Cl in 81% and 86% isolated yield, respectively. Depending on the hexachlororhenate:Na ratio, either carbonyl derivative can be obtained almost exclusively. (C) 1997 Elsevier Science S.A.