Abstract A variety of N -(1-methoxyalkyl)amides react with benzotriazole in the presence of PPh 3 ·HBF 4 and organic bases (Hunig's base, DBU or DABCO) or solid-state-supported bases (SiO 2 -Pip or IRA-67) in CHCl 3 to give N -[1-(benzotriazol-1-yl)alkyl]amides in good yields. The most convenient and efficient procedure for obtaining N -[1-(benzotriazol-1-yl)alkyl]amides consists, however, of the addition of benzotriazole sodium salt to a solution of crude 1-( N -acylamino)alkyltriphenylphosphonium salt, obtained in situ from N -(1-methoxyalkyl)amides and PPh 3 ·HBF 4 . A combination of these reactions with the recently described electrochemical decarboxylative α-methoxylation of N -acyl-α-amino acids in the presence of SiO 2 -Pip enables an effective two-pot transformation of N -acyl-α-amino acids to N -[1-(benzotriazol-1-yl)alkyl]amides.