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3,6-Diarylidene-2,5-piperazinediones(2)and 3-alkylidene-6-arylidene-2,5-piperazfnediones(6)were synthesized from diacetyl-2,5-piperazinedione(1)under solid-liquid phase transfer catalyticconditions.2 could be easily convered to a-amino acid by reducing with zinc powder and hydrolyzingwith concentrated hydrochloric acid.The effect of different phase transfer catalysts and reaction con-ditions were studied.