This chapter describes the procedure for synthesis of N‐Boc‐N‐hydroxymethyl‐L‐phenylalaninal and methyl trans‐oxazolidine‐5‐carboxylate, chiral synthons for threo‐β‐amino‐α‐hydroxy acids. 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.