Lower and higher homologs, L-2-amino-4-(p-methoxyphenyl) butanoic acid (L-Amb) and L-2- amino-6-(p-methoxyphenyl) hexanoic acid (L-Amh), of L-2-amino-5-(p-methoxyphenyl) pentanoic acid were prepared by optical resolution of N-acetyl-DL-Amb and of N-acetyl-DL- Amh with Aspergillus acylase. N-Acetyl-DL-Amb or N-acetyl-DL-Amh was synthesized from [2-(p-methoxyphenyl) ethyl or butyl](acetamido) malonic acid by heating with p-xylene.