The use of polystyrene-supported hydroxamic esters in the synthesis of amides is illustrated. The crosslinking agents used were divinylbenzene (DVB) and ethyleneglycol dimethacrylate (EGDMA). The reagent was found to selectively acylate amines and amino acids to give the corresponding amides. Acyl transfer reagents derived from EGDMA-crosslinked polystyrene support were found to be superior to those based on DVB-crosslinked polystyrene support in terms of functional group capacity and reactivity. The spent polymeric reagent could be regenerated by a simple reaction, without considerable loss in activity.