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The dealkylation of phosphaisocoumarin esters was studied under various conditions. An effective way to synthesize phosphaisocoumarin acids was developed via the reaction of phosphaisocoumarin esters with Me 3 SiBr in chloroform followed by treatment with methanol, or with Me 3 SiCl and NaI in acetonitrile followed by hydrolysis, under mild conditions in good to excellent yields.