Layered brucite was synthesized at room temperature and, after characterization, was reacted in a closed flask with either ethylene glycol or glycerol. Powder X-ray diffraction patterns have shown that new compounds with interlayer expansions were obtained. New bands attributed to grafting of ethylene glycol and glycerol into the interlayer surface of brucite were detected by FTIR. XPS spectroscopy and thermal analyses (TG/DSC) have shown that nearly all of the hydroxide groups of the layers were replaced by either ethylene glycol or glycerol through Mg-O-C bonds.