Abstract: | Efficiency and structural specificity earmark the reaction of phosphonium ions 1 with cyclic acetals and ketals to yield 1,3,2‐dioxaphospholanium ions 2 Eq. (1)]. Potential applications of this reaction are in monitoring trace levels of organophosphorus esters and in developing novel carbonyl deprotection agents. R=OCH3, CH3; R1=H, CH3; R2=CH3, C6H5; R3=H, CH3. |