Next, we were interested to evaluate this mild protocol with 1.3-dioxolane 3, 1,3-dioxane 4, and with 1,3-oxathiane 5. As it could be seen in Scheme 1, by using TMSCl/NaI in CH3CN under conditions A (seen in entry 7 of Table ), we observed a clean and complete deprotection of ketals 3 and 4 as well as 1.3-oxathiane 5 into ketones (93 to 97%). For comparison, Jung reported that TMSI in CHCl3 deprotected ethylene ketals into ketones but with very low yields (20 %) and that TMSI did not react with thioketals after 24 h of mixing at 75 °C. Encouraged by these results and by the simplicity of this process, the deprotection of a variety of thioacetals 1 was carried out with the TMSCl/NaI association in CH3CN for 24 h. Table summarizes the results of this study achieved using 10 eq of TMSCl/NaI at rt (conditions A) or 20 eq of TMSCl/NaI at 60 °C (conditions B) for less cooperative substrates.