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This approach facilitates the efficient synthesis of ester-substituted dioxodihydrodibenzothiazepine derivatives in the absence of photocatalysts and transition metals. The methodology features a broad substrate scope, operational simplicity, excellent functional group tolerance, mild reaction conditions, and scalability. Mechanistic experiments proved that the reaction involves a pathway that includes the formation of the carbon dioxide radical anion (CO2\u2022\u2013) from formate. 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