Five novel benzenoids, polycarpamines A-E (1-5), with rare, sulfur-containing functional groups, have been isolated from the solitary marine ascidian Polycarpa auzata. The structures of these compounds were determined primarily through interpretation of their NMR characteristics and mass spectral fragmentation patterns. Polycarpamine B (2) exhibited significant antifungal activity in vitro against Saccharomyces cerevisiae and Candida albicans.