Synthesis and solid-state NMR studies of p-vinylbenzylphosphonic acid

P-Vinylbenzylphosphonic acid (2) was synthesized and crystallized in two phases A and B. The latter phase was easily converted into the former. Both phases were investigated by IR and solid-state (31)P and (1)H NMR spectroscopy, and X-ray crystallography. The use of recently developed NMR methods has enabled us to increase the usually poor resolution of solid-state (1)H spectra. This gave additional insights on the proton environments. In particular, two dimensional 2D (1)H-(31)P heteronuclear correlation (HETCOR) experiments, incorporating a Lee-Golburg homonuclear decoupling scheme, allowed description of the mixture of phase A and B.