The syntheses and properties of p-nitrobenzyl diazoacetyl-glycinate (VI), p-nitrobenzyl p-(p-methoxyphenylazo)-benzyloxycarbonyl-glycyl-glycollyl-glycinate (II) and p-nitrobenzyl p-phenylazo-benzyloxycarbonyl-glycyl-glycollyl-glycinate are described. These compounds have been prepared as intermediates for the synthesis of other depsipeptides.