This laboratory experiment provides undergraduate students enrolled in organic chemistry the opportunity to design and synthesize their own peptide, which is then tested for antimicrobial activity. After reading a primary scientific paper on antimicrobial peptides, students design and synthesize their own hexapeptide that they hypothesize will have antimicrobial activity. The students characterize their products by analyzing liquid chromatography-mass spectrometry and antimicrobial bioassay data for their synthesized peptide. The students are able to complete the synthesis and prepare their samples for analysis in three 3-4 h lab periods; instructors perform LC-MS and a bioassay with the peptides and provide data to students for analysis. This exercise is flexible and can be altered to include students performing the bioassay, or to meet different time constraints or target student populations. This experiment allows students to increase their knowledge of solid phase peptide chemistry and gain experience with developing and testing hypotheses through experimental design.