The condensation of the N-(benzyloxycarbonyl)-D-glutamic acid 5-benzyl ester (I) with N-(3-methoxypropyl)-N-pentylamine (II) by means of ethyl chloroformate and triethylamine in THF gives the corresponding amide (III), which is debenzylated by hydrogenation over Pd/C in methanol, yielding compound (IV). Finally, the free amino group of (IV) is acylated with 3,4-dichlorobenzoyl chloride (V) by means of NaOH in water to give dexloxiglumide.