Abstract

A convenient procedure for the synthesis of the rhenium carbonyls Re2(CO)10 and Re(CO)5 Cl is reported. Sodium reduction of the easily available K2ReCl6, under CO presssure (2400 psi, 280°C (external temperature), THF as solvent) affords Re2(CO)10 and Re(CO)5Cl in 81% and 86% isolated yield, respectively. Depending on the hexachlororhenate:Na ratio, either carbonyl derivative can be obtained almost exclusively. © 1997 Elsevier Science S.A.