Mechanism of Vinylic and Allylic Carbon−Fluorine Bond Activation of Non-Perfluorinated Olefins Using Cp*2ZrH2

Abstract
Cp*2ZrH2 (1) (Cp* = pentamethylcyclopentadienyl) reacts with vinylic carbon−fluorine bonds of CF2CH2 and 1,1-difluoromethylenecyclohexane (CF2C6H10) to afford Cp*2ZrHF (2) and hydrodefluorinated products. Experimental evidence suggests that an insertion/β-fluoride elimination mechanism is occurring. Complex 1 reacts with allylic C−F bonds of the olefins, CH2CHCF3, CH2CHCF2CF2CF2CF3, and CH2C(CF3)2 to give preferentially 2 and CH3−CHCF2, CH3−CHCF−CF2CF2CF3, and CF2C(CF3)(CH3), respectively, by insertion/β-fluoride elimination. In the reactions of 1 with CH2CHCF3 and CH2CHCF2CF2CF2CF3, both primary and secondary alkylzirconium olefin insertion intermediates were observed in the 1H and 19F NMR spectra at low temperature. A deuterium labeling study revealed that more than one olefin-dihydride complex is likely to exist prior to olefin insertion. In the presence of excess 1 and H2, CH2CHCF3 and CH2CHCF2CF2CF2CF3 are reduced to propane and (E)-CH3CH2CFCFCF2CF3, respectively.

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