Synthetic studies on ethyl α, β-unsaturated β-nitrocarboxylates (IV) through two routes are described. Ethyl α-hydroxy-β-nitrocarboxylates (II) obtained by the reactions of ethyl α, β- unsaturated carboxylates with fuming nitric acid or by those of nitroparafins with ethyl glyoxylate, were treated with acetic anhydride to afford ethyl α,-acetoxy-β-nitrocarboxylates (III), which were subsequently converted into IV by treatment with bases used as catalysts. ...