The synthesis of four 2-amino-1, 3-alkanediols (5) has been described. 2-Nitroethanol (1) was condensed with aliphatic aldehydes (2) in the presence of sodium methoxide in methanol to give aci. sodium salts of 2-nitro-1, 3-alkanediols, (3), which were decomposed with an acid (aq. HCl) to free 2-nitro-1, 3-alkanediols (4). The nitro group of (4) was reduced with Zn-HCl in ethanol. The resulting (5) were purified by column chromatography, and their structures were confirmed by elemen-tal analyses and IR spectra of (5), and by MS spectra of O, O-bis (trimethylsilyl) derivatives of (5).