A comparative synthesis of the classic difficult sequence ACP(65-74) on 2% crosslinked JandaJel and 1% crosslinked polystyrene-divinylbenzene, (PS-DVB, Merrifield resin) by Boc/benzyl chemistry is presented. The JandaJel batch used was of nearly double the loading of PS-DVB, yet 12.2% less of the des-Val 6 5 contaminant was observed in the JandaJel synthesis. These results suggest that the increased swelling of the JandaJel resin relative to traditional Merrifield resin afforded a higher yield of the pure peptide by permitting greater solvent-mediated disruption of secondary structure in the resin-bound peptide.