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A Modern Twist to a Classic Synthetic Route: Ph<sub>3</sub>Bi-Based Redox Transmetalation Protolysis (RTP) for the Preparation of Barium Metalorganic Species
This
paper reports advances in redox transmetalation/protolysis (RTP) utilizing
the readily available Ph<sub>3</sub>Bi for the synthesis of a series
of barium metal-organic species. On the basis of easily available
starting materials, an easy one-pot procedure, and workup, we have
obtained BaL<sub>2</sub> compounds (L = bis(trimethylsilyl)amide,
phenyl(trimethylsilyl)amide, pentamethylcyclopentadienide,
fluorenide, 2,6-di-isopropylphenolate, and 3,5-diphenylpyrazolate)
quantitatively by sonication of an excess of barium metal with triphenylbismuth
and HL in perdeuterotetrahydrofuran, as established
by NMR measurements. Rates of conversion are affected by both p<i>K</i><sub>a</sub> and bulk of HL. Competition occurs from direct
reaction of Ba with HL, thereby enhancing the overall conversion,
the effect being pronounced for the less bulky and more acidic ligands.
Overall, the method significantly adds to the synthetic armory for
barium metal-organic/organometallic compounds