In situ high pressure NMR study of the direct synthesis of LiAlH4

27Al and 7Li wide-line NMR spectroscopy incorporating a high pressure NMR apparatus has allowed the first in situ study of the solvent mediated, direct synthesis of an alanate, thus overcoming the dearth of analytical techniques available to study phenomena occurring in a pressurised slurry. In contrast to the decomposition reaction, the elucidated hydrogenation pathway does not proceed through the hexahydride intermediate.