Organometallic Synthesis as a Continuous Process: The Synthesis and Isolation of Cr(CO)5(η2-C3H6) and (C5R5)Mn(CO)2(η2-C3H6) (R = H and Me) from Superheated Liquid Propene

Abstract

(C5R5)Mn(CO)2(η2-C3H6) (R = H and Me) and Cr(CO)5(η2-C3H6) have been synthesized by UV photolysis of CpMn(CO)3 and Cr(CO)6 in liquid propene at 25 °C and 2100 psi pressure and by the thermal reaction of Cp*Mn(CO)2(EVE) (EVE = ethyl vinyl ether) with propene. The propene complexes are precipitated by rapid expansion through a back pressure regulator. The precipitation leads to finely divided solid materials. Although these contain some residual starting materials, none of the compounds have previously been isolated as solids. All three compounds are significantly more stable in the solid state than in solution. The Cp* complex appears to be thermally less stable than the Cp analog.