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Phthalide is an important scaffold found in several biologically active compounds. Therefore, effective methods for the synthesis of phthalides are strongly desired. Herein, we describe the metal‐free synthesis of 3‐substituted phthalides by the reductive hydroiodination of 2‐alkynylbenzoates through an I2/PPh3/H2O‐triggered cascade reaction. A variety of 3‐substituted phthalides were synthesized...
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