SUMMARY3,4,5-Trimethoxy-'Hg-, 4-metho~y-3,5-dimethoxy-~H~-, and 4-hydroxy-3,5-dimethoxy-*H6-benzoic acids were prepared from g-propyl 3,4,5-trihydroxybenzoate (n-propyl gallate) by means of appropriate alkylationhydrolysis sequences employing iodor~iethane-~H~ or dimethyl-'H6-sulfate as the deuterium source. similarly prepared from ethyl 4-hydroxy-3,5-dirnethoxybenzoate.labeled trimethoxybenzoic acids were converted to the corresponding 2H-labeled reserpines by condensation of the acid chlorides with methyl reserpate in pyridine according to the classical procedure. The labeled reserpine analog methyl 18-0-(4-hydroxy-3,5-dimethoxy-2H6)benzoyl reserpate was likewise prepared from 4-hydro~y-3,5-dimethoxy-~H~-benzoic acid via the intermediate methyl 18-0-(4-ethoxycarbonyloxy-3,5-dimethoxy-*H~-benzoy1)reserpate (syrosing~pine-~H~). The isotopic purity of each compound exceeded 99 atom percent ZH.