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The first general synthesis of bis‐α‐acyloxy‐1,4‐ and ‐1,5‐diketones has been accomplished in a catalytic oxidative opening of bis‐acylated THF and THP (tetrahydropyran) diols, which were synthesised by osmium‐ or ruthenium‐catalysed oxidative cyclisation of 1,5‐ and 1,6‐dienes. The overall sequence corresponds to the regioselective double ketoacyloxylation of the starting diene. The synthesised bis‐α‐acyloxy‐1,5‐dicarbonyl...
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