This chapter describes the procedure for preparation of a Donor‐Acceptor Stenhouse Adduct (DASA): 5‐((2z,4e)‐5‐(Diethylamino)‐2‐hydroxypenta2,4‐dien‐1‐ylidene)‐2,2‐dimethyl‐1,3‐dioxane‐4,6‐dione. 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. Since their discovery, DASA's promising properties – visible light activation, high extinction coefficient, negative photochromicity, large volume and polarity change – have enabled a number of applications including drug release, phase transfer, programmable adhesion, photothermally controlled flow, and amine and heat sensing.