<jats:title>Abstract</jats:title><jats:p>From the stem bark of <jats:italic>Aspidosperma discolor</jats:italic> A. DC. (–)‐reserpiline, (–)‐isoreserpiline, (+)‐yohimbine, (–)‐10‐methoxy‐geissoschizol and (–)‐10‐methoxy‐dihydrocorynantheol (major alkaloids) and (–)‐isoreserpiline‐ψ‐indoxyl, AD‐V (–)‐β‐yohimbine, (+)‐haplocidine, (+)‐desmethylaspidospermine and (–)‐demethoxy‐aspidospermine (minor alkaloids) have been isolated.