“…L-Lactide (LA; TCI; >98.0%) was recrystallized from 1,4-dioxane and then toluene before being dried for more than 3 h. 1,3-Dioxepane (DOP), 2-methyl-1,3-dioxane (MDOX), MDOP, and 2,2-dimethyl-1,3-dioxepane (DMDOP) were synthesized according to previously reported procedures. [28][29][30] ε-Heptanolactone (ε-HepL) was synthesized by Baeyer-Villiger oxidation according to previously reported procedures. 31,32 EtSO 3 H (Aldrich; 95%), PhSO 3 H (TCI; >98.0%), p-toluenesulfonic anhydride (Ts 2 O; Aldrich; 97%), trifluoromethanesulfonic acid (TfOH; Aldrich; >99.0%), bis(trifluoromethanesulfonyl)imide (Tf 2 NH; Wako; 98.0+%), and Ti(OBu) 4 (Alfa Aesar; 99+%) were used without further purification after preparing stock solutions in CH 2 Cl 2 .…”