ZnO nanoparticles of different sizes, from 20 to 200 nm in length, and morphologies, nanorods and coral-like structures, were synthesized via a simple one-pot synthesis by refluxing an oversaturated solution of zinc acetylacetonate hydrate in 1-butanol and isobutanol. On the basis of H-1 and C-13 NMR experiments, the reactions in both alcohols were found to proceed via the alcoholytic C-C cleavage of the acetylacetonate ligand, followed by the hydrolytic formation of the reactive Zn-OH intermediate from the water molecules present in the precursor hydrate species and/or those released during the condensation cycle. The zinc acetylacetonate conversion into ZnO in isobutanol is significantly slower than in the case when 1-butanol was used as both the medium and the reagent. FE-SEM studies showed that in 1-butanol the growth of the rod-shaped particles occurs via the agglomeration of ZnO primary particles that are less than 10 nm in size. The morphology of the particles formed in the isobutanol is time dependent, with the final coral-like structures developing from initially formed bundle-like structures. (C) 2010 Elsevier Inc. All rights reserved.