The presence of alkaloids was chromatographically demonstrated in seven species of Coryphantha. By using preparative chromatographic techniques, N‐methyl‐3,4‐dimethoxy‐β‐phenethylamine, N‐methyl‐4‐methoxy‐β‐phenethylamine, N‐methyltyramine, and N,N‐dimethyltyramine (hordenine) were isolated from extracts of C. cornifera (DC.) Br. and R. var. echinus (Engelm.) L. Benson. In addition, two new cactus alkaloids, N‐methyl‐4‐hydroxy‐β‐methoxy‐β‐phenethylamine (β‐O‐methylsynephrine) and 4‐methoxy‐β‐hydroxy‐β‐phenethylamine, were identified spectroscopically in extracts of this species. Copyright © 1972 Wiley‐Liss, Inc., A Wiley Company