Two new alkaloids were isolated from the Mexican cactus Coryphantha calipensis H. Bravo. Based on chemical and spectroscopic data, their structures were determined as (−)‐N‐methyl‐3,4‐dimethoxy‐β‐O‐methoxyphenethylamine [(−)‐β‐O‐methylnormacromerine] and (−)‐N,N‐dimethyl‐3,4‐dimethoxy‐β‐methoxyphenethylamine [(−)‐β‐O‐methylmacromerine]. The isolation of (−)‐normacromerine and N‐methyl‐3,4‐dimethoxyphenethylamine from this species is also reported. Copyright © 1974 Wiley‐Liss, Inc., A Wiley Company