Abstract: In order to disclose the role of N-glycosyl amides-containing proteins in the life process, an efficient separation and purification ofα-/β- isomers were urgently required. This paper reported a synthesis and purification of two pairs of α-/β-furanoribosyl amide, 6a/6b and 9a/9b. The results show the important role of basic developing solvents to separate α- and β-isomers by thin layer chromatography (TLC). And a high ΔR_f of 0.24 between α-and β-isomers (9a/9b) are achieved, which lead to their easy peperation by flash column chromatography.