Cleavage of aryl alkyl ethers was conducted in a one-pot onestage manner by mixing the ethers, aluminum and iodine in acetonitrile without the in situ preparation of aluminum triiodide in advance. For ethers bearing acid-labile functional groups such as allyl, alkenyl and carbonyl, an acid scavenger (calcium oxide, 1,3-diisopropylcarbodiimide or dimethyl sulfoxide) was used to prevent side-reactions. This one-pot protocol is efficient and convenient for the removal of methyl, ethyl, isopropyl and tert-butyl groups from typical aryl alkyl ethers, catechol monomethyl and dimethyl ethers, and is compatible with a variety of functional groups including alkenyl, alkyl, allyl, amido, cyano, formyl, halogen, keto and nitro group. Methyl 2-anisate and eugenol acetate were exhaustively deprotected by the method that afforded salicylic acid and hydroxychavicol, respectively.