N-[N-(3,3-dimethylbutyl)-L- a -aspartyl]-L-phenylalanine 1-methyl ester is produced by hydrolyzing a bisulfite adduct of 3, 3-dimethylbutyraldehyde with a base in a solvent, or by regenerating 3, 3-dimethylbutyraldehyde from a hydrazone, a semicarbazone or an oxime of 3,3-dimethylbutyraldehyde by acidic hydrolysis or oxidative cleavage in a solvent, or by hydrolyzing a trimer of 3,3-dimethylbutyraldehyde with an acid in a solvent. The production methods are efficient and low cost, as compared with conventional N-[N-(3,3-dimethylbutyl)-L-±-aspartyl]-L-phenylalanine 1-methyl ester synthesis.
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