A copper-catalyzed aminoacyloxylation of unactivated alkenes of unsaturated hydrazones is achieved by using various commercially available carboxylic acids as the acyloxylating reagents and di- tert-butyl peroxide (DTBP) as the oxidant. By using this method, a sequence of structurally diversiform acyloxyl-substituted pyrazolines are efficiently synthesized. Significantly, many carboxyl-containing drugs and bioactive molecules with unprotected functional groups are compatible in this reaction.