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Enantioselective hydrolysis of methyl ester of (±)-C75 was successfully accomplished by means of Acylase I from Aspergillus to afford (2R,3S)-(+)-C75 with 96% e.e. The unreacted methyl ester was recovered with >99% e.e. This latter compound was either chemically or enzymatically hydrolyzed to furnish (2S,3R)-(-)-C75 with >99% e.e.