Acetylacetonates were prepared electrochemically in good yield using the pure liquid ligand, acetylacetone, as the solvent, in which the supporting electrolyte, tetra‐n‐butyammonium hexafluorophosphate, was dissolved; the metal of interest served as the electrodes. The products were characterized by UV‐visible spectrometry (color) and mass spectrometry. Both a lower, M(AcAc)2, and a higher, M(AcAc)3, oxidate state were formed for the cobalt and manganese systems; the identity of the product(s) could be biased by a careful choice of the potential used for the synthesis.
We gratefully acknowledge the support of the Robert A. Welch Foundation in the form of a scholarship (SRL) and to the University Cooperative Society for the purchase of the metals used in this work.