Peptides are advantageous as therapeutic vectors in PRRT due to their small size, favorable pharmacokinetics, high binding affinity, low immunogenicity and toxicity, and minimal off-target binding. This case study presents a manufacturing process for DOTAGA-Labeled urea-based peptide PSMA inhibitor API, DOTAGA-(I-y)fk(Sub-KuE). Multigram-scale process development and GMP manufacturing was completed in only ten months. Through optimized synthesis, cleavage, and purification an overall yield of >65% (>98% purity) was achieved.