Nickel Catalyzed Carbonylation/Carboxylation Sequence via Double CO 2 Incorporation.

A carbonylation-carboxylation synthetic sequence, via double CO 2 fixation, is described. The productive merger of a Ni-catalyzed cross-electrophile coupling manifold, with the use of AlCl 3 , triggered a cascade reaction with the formation of three consecutive C-C bonds in a single operation. This strategy traces an unprecedented synthetic route to ketones under Lewis acid assisted carbon dioxide valorization. Computational insights revealed a unique double function of AlCl 3 , and labeling ( 13 CO 2 ) experiments validate the genuine incorporation of CO 2 in both functional groups.