A number ofN-acylalkylenediamines were synthesized in high yields byin situ monoamidation of car☐ ylic acids with diamines. The amidation reactions were carried out simply by heating the substrates at 110° C for 5–24 h in the presence of HMDS. HMDS- promotedin situ amidation reactions are generally applicable to the synthesis ofN- acylalkylenediamines.