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Recent studies by Armstrong, McMillan, and Shaw(1) have shown that a major metabolite of norepinephrine and epinephrine found in human urine is 3-methoxy-4-hydroxymandelic acid. Subsequently it was shown by Axelrod (2) that the 3-hydroxy position of both norepinephrine and epinephrine can be methylated by animal tissues to yield the corresponding 3-methoxy analogs. The 3-methoxy analog of epinephrine (ME) was also reported to be present in rat urine (2). Since the conversion of catecholamines to their methoxy analogs may play some role in the physiology of these agents, it seemed important to determine whether these substances exist in man.