Carbosylate Method for the Synthesis of Metal carbonyls

The results of obtaining metal carbonyls are presented. Iron and nickel carbonyls are obtained by carbonylation of metal powders. A reducing agent is required to obtain metal carbonyls. Depending on the nature of the metal or the type of its compound, different types of reducing agents are required. When nickel bis(trifluoroacetate) is heated to 200°C in a high-pressure carbon monoxide atmosphere (200‒300 atm or 20‒30 MPa), nickel tetracarbonyl is formed in high yield. Probably, bis(perfluoromethyl) nickel is formed initially, which is rapidly carbonylated under the process conditions. Under conditions similar to nickel, thermal decarboxylation of iron trifluoroacetate (temperature 200‒210°C and pressure 250‒300 atm or 25‒30 MPa) occurs with the formation of iron pentacarbonyl in high yield.