Abstract
Abstract1,3‐cyclohexanedione‐2‐13C was prepared by intramolecular Claisen condensation of methyl 5‐oxohexanote‐6‐13C with sodium methoxide. Formation of the ketoester starting material involved treatment of a mixed dicarboxylic anhydride with an isotopicallylabelled Grignard reagent, methyl‐13C magnesium iodide. Dehydrogenation of carbon‐13 labelled cyclohexanedione over a palladium/carbon catalyst produced 1,3‐dihydroxybenzene‐2‐13C. Chlorination and bromination of dihydroxybenzene in aqueous solution yielded isotopically‐labelled chloroform and bromoform, each having enriched carbon‐13 contents equivalent to that of the organic substrate.
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