NiO nanoparticles with an average size of 12 nm and a high specific surface area of 88.5 m 2/g were easily prepared via the thermal decomposition of the complex Ni(dmgH) 2 and were characterized by TGA, XRD, FT-IR, TEM and BET surface area measurement. This nanosized transition metal oxide was used as a new heterogeneous catalyst for the reduction of nitroarenes under microwave irradiation. The efficient and selective reduction of aromatic nitro compounds into their corresponding amines was observed by using ethanol as a hydrogen donor (reducing agent) and KOH as a promoter under microwave irradiation. This highly regio- and chemoselective method is fast, simple, inexpensive, high yielding, clean and compatible with several sensitive functionalities, such as halogens, –OH, –OCH 3, –CHO, –COCH 3, –COOH, –COOEt, –CONH 2, –CN, –CH CH 2 and –NHCOCH 3. This method is suitable for the large scale preparation of different substituted anilines as well as other arylamines. In addition, the catalytic activity of nanosized NiO is higher than that of the bulk sample.