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About 1 kg of racemic <jats:italic>N<\/jats:italic>\u2010carbobenzoxy\u2010<jats:italic>tert<\/jats:italic>\u2010leucine was resolved on the cellulose\u2010based phase Chiralcel OD using a mixture of heptane\/ethanol and 0.1% of trifluoroacetic acid modifier as the mobile phase, while 520 g of the N\u2010Boc\u2010<jats:italic>tert<\/jats:italic>\u2010leucine\u2010benzylester was resolved on the amylose\u2010based phase Chiralpak AD with a mixture of heptane\/2\u2010propanol as the mobile phase. In both instances the corresponding enantiomers were obtained in high yield and high optical purity. 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