Synthesis of 2-substituted adenosines of formula (I) using 2-nitro pentabenzoyl adenosine, or 2-nitro pentaacetyl adenosine, as intermediate is described: Formula (I) wherein R=C.sub.1-6 alkoxy (straight or branched), a phenoxy group (unsubstituted, or mono-, or di-substituted by halo, amino, CF.sub.3--, cyano, nitro, C.sub.1-4 alkyl, or C.sub.1-4 alkoxy), a benzyloxy group (unsubstituted, or mono-, or di-substituted by halo, amino, CF.sub.3--, cyano, nitro, C.sub.1-6 alkyl, or C.sub.1-6 alkoxy), or a benzoyl group (unsubstituted, or mono-, or di-substituted by halo, amino, CF.sub.3--, cyano, nitro, C.sub.1-6 alkyl, or C.sub.1-6 alkoxy). The methods provide improved yield and purity of product. ##STR00001##