5'-Deoxy-5-fluorouridine (5'-DFUR) has been obtained in high yield and purity by stereospecific condensation of the anomeric 5-deoxy-1, 2, 3-tri-O-acetyl-tl-ribofuranose with bis (trimethylsilylated)-5-fluorouracil in the presence of trimethylsilyl trifluoromethanesulfonate, and by subsequent cleavage of the acetate protecting groups. A minor by-product of the synthesis, the a-anomeric nucleoside is produced by a (j?+ a)- ...