A new, simple route leading to layered rare-earth hydroxy nitrates was developed. The pH-independent procedure uses ethanol containing alkali-metal hydroxide (KOH, RbOH, or CsOH) as a solvothermal medium. Two new, layered rareearth hydroxy nitrates (LRHs), Nd 2 (OH) 5 NO 3 ·nH 2 O and La 2 (OH) 5 NO 3 ·nH 2 O, were prepared by this nonaqueous solvothermal reaction. Because the RE = Nd and La members have not yet been synthesized in an aqueous system, the successful synthesis of these compounds implies the completion of the RE 2 (OH) 5 NO 3 ·nH 2 O (RE = rare earths) series. The typical properties of a layered structure was demonstrated by ready ion-exchange reactions between NO 3 -and some or-