O-Methyl hydroxamic acids, readily available from carboxylic acids, are found to be extremely reactive for P-C-H activation by Pd(OAC)(2). This reactivity is exploited to develop the first example of cross-coupling sp(3) C-H bonds with sp(3) boronic acids. Air was shown to be a suitable stoichiometric oxidant for the catalytic oxidative coupling reaction. A biologically active natural product is readily converted to its novel analogues through this coupling reaction.