Analysis of illicit methamphetamine samples revealed the presence of a hitherto unreported impurity. This was identified as N-acetylmethamphetamine by synthesis and GC-MS. This impurity is believed to arise by transesterification of methamphetamine during reflux with propyl acetate. Other circumstantial evidence and intelligence data indicate that propyl acetate was used to increase yields of methamphetamine hydrochloride by azeotropic removal of water remaining after salt formation with aqueous hydrochloric acid.