Abstract
<jats:title>Abstract</jats:title> <jats:p>This chapter describes the procedure for the preparation of hindered aniline cyanH and explains the application in the allyl‐ni‐catalyzed α,β‐dehydrogenation of carbonyls. The α,β‐dehydrogenation of carbonyl compounds introduces a synthetic handle that allows for a wide variety of transformations. Development of the nickel‐catalyzed dehydrogenation methodology addresses current limitations of allyl‐palladium‐catalyzed dehydrogenation chemistry. The identity of the base used in these reactions had an important effect on the outcome of the reactions. The chapter presents some of the important points to be considered, the conditions that need to be maintained, characterization data, and the reagents required, as well as the techniques used and the equipment setup that are vital to carrying out the process. It also describes the hazards associated with working with chemicals and the ways to deal with these hazards.</jats:p>