Reactions of diethyl α-hydroxyphosphonates have been under investigation in our laboratory in recent years. [10] Along this line, recently we have introduced [Cu(OTf) 2 ] as a mild and efficient catalyst for the silylation of α-hydroxyphosphonates with HMDS. [10d] A recent report on the acetylation of traditional hydroxy functional groups with Ac 2 O catalyzed by Cu(OTf) 2 [11] prompted us to apply this Lewis acid catalyst for direct acetylation of diethyl α-hydroxyphosphonates. ...