Unusual lability and stability of haloarenes in the presence of n-BuLi

ORGN 165

DW. Slocum, donald.slocum@wku.edu, Troy Reece, Jared Bolton, Seth Parmley, and Paul Whitley. Department of Chemistry, Western Kentucky University, 1906 College Heights Blvd., Bowling Green, KY 42101
Our published observation of the stability of chlorobenzene to the presence of n-BuLi in cyclohexane has led to several further investigations. In cyclohexane p-chloroanisole (p-ClA) slowly undergoes metalation ortho to the methoxy group. Under identical conditions p-fluoroanisole (p-FA)undergoes ortho-lithiation more rapidly. Little hint of a competing benzyne reaction is observed. The order of metalation reactivity when compared to that of anisole (A) is p-FA >p-CIA> A for a given set of conditions, including elevated T. In addition to a conventional electronegativity rationale for this order, an explanation based on a contribution by an opposing-π-resonance effect will be presented. Several derivatives of these metalated intermediates have been prepared. When ortho-lithiodimethylaniline (o-LiDMA) in cyclohexane is treated with o-IA, the reaction proceeds in the direction shown.

o-LiDMA + o-IA → o-IDMA + o-LiA

There is little or no evidence of the presence of an equilibrium. Implications regarding the relative neoleophilicity/basicity of o-LiDMA and o-LiA will be discussed.