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A novel, facile, and versatile microwave-assisted method of high-yield synthesis of layered rare earth hydroxo compounds (LRHs) is proposed. Layered yttrium hydroxonitrates synthesized by the microwave-assisted technique crystallize in the form of thin hexagonal plates aggregated into spheroidal particles. Depending on the conditions of microwave-assisted hydrothermal synthesis, the formation of several phases differing in interplanar spacing along the [00l] direction is possible. The materials obtained are shown to possess good anion-exchange properties. This work provides a route to large-scale synthesis of LRH-based advanced materials.