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An efficient method for the preparation of 1,3-dithiolanes of aliphatic and both activated and deactivated aromatic carbonyl compounds with 1,2-ethanedithiol in the presence of a catalytic amount of inexpensive, easily recyclable, monodispersed, chemoselective Ni-nanoparticles having high TON and TOF is reported. An efficient method for the chemoselective thioacetalization of ketones in the presence of aldehydes using Ni-nanoparticles is also reported in this article. Our reaction is kinetically controlled and the method is relatively expedient, avoids the use of cost-prohibitive reagents, high temperatures and leads to excellent yield. Selective Protection of Carbonyl Compounds Over Nano-sized Nickel Catalysts Ajeet Kumar,a Santosh Kumar,a Amit Saxena,a Arnab De,b Subho Mozumdara* aDepartment of Chemistry, University of Delhi, Delhi, 110007, India; b Department of Chemistry, Indiana University, Bloomington, USA; subhoscom@yahoo.co.in An efficient method for the preparation of 1,3-dithiolanes of aliphatic and both activated and deactivated aromatic carbonyl compounds with 1,2-ethanedithiol in the presence of a catalytic amount of inexpensive, easily recyclable, monodispersed, chemoselective Ni-nanoparticles having high TON and TOF is reported. We report an efficient method for the chemoselective thioacetalization of ketones in the presence of aldehydes using Ni-nanoparticles. Our reaction is kinetically controlled and the method is relatively expedient, avoids the use of cost-prohibitive reagents, high temperatures and leads to excellent yield. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]