The isolation of N-methyl-dioncophylline A and N-methyl-7-epi-dioncophylline A from Ancistrocladus abbreviatus is described. Atrop-diastereomer resolution was achieved analytically on a chiral chromatographic phase, and preparatively after esterification with a chiral carboxylic acid. Structural elucidation assisted by partial synthesis is reported and chemotaxonomic implications of this first isolation of Dioncophyllaceae alkaloids from an Ancistrocladus species are discussed. © 1991.