Synthesis of Bicyclo[n.1.0]alkanes by a Cobalt‐Catalyzed Multiple C(sp3)−H Activation Strategy

A cobalt‐catalyzed dual C(sp³)−H activation strategy has been developed and it provides a novel strategy for the synthesis of bicyclo4.1.0]heptanes and bicyclo3.1.0]hexanes. A key to the success of this reaction is the conformation‐induced methylene C(sp³)−H activation of the resulting cobaltabicyclo4.n.1] intermediate. In addition, the synthesis of bicyclo3.1.0]hexane from pivalamide, by a triple C(sp³)−H activation, has also been demonstrated.