The condensation of 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide with a variety of nitro alcohols led to nitroalkyl β-D-glucopyranoside tetraacetates. The following nitro alcohols were employed: 3-nitro-1-propanol, 2-nitro-1-propanol, 1-nitro-2-propanol, 2-nitro-1-butanol, 2-nitro-3-pentanol, and 2-methyl-2-nitro-1-propanol. The free 3-nitropropyl and 2-methyl-2-nitropropyl glycosides were obtained from their tetraacetates by deacetylation with sodium methoxide, whereas methanolysis catalyzed by methyl p-toluenesulfonate was employed for deacetylation of the other tetraacetates. Evidence for the presence of epimers in glycosides having a chiral center in the aglycon was obtained. Physical data of synthetic 3-nitropropyl β-D-glucopyranoside agreed with those of miserotoxin, the poisonous principle recently isolated from Astragalus miser varieties.