Abstract
<jats:title>Abstract</jats:title> <jats:p> This chapter describes the procedure for reductive deuteration of ketones with magnesium and D <jats:sub>2</jats:sub> O for the synthesis of α‐deutero‐o‐methyl‐benzhydrol. It 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. The chapter also describes the hazards associated with working with chemicals and the ways to deal with these hazards. Reductive deuteration of carbonyl compounds is the most straightforward process to deliver α‐deuterated alcohols. In terms of a practical and general synthesis of α‐deuterated alcohols in large quantities, the umpolung strategies which use D <jats:sub>2</jats:sub> O as the deuterium source have great advantages in price, supply, and safety. </jats:p>