Provided is a process for preparing gemcitabine or a salt thereof, which preferably includes selectively precipitating the .beta.-anomer of a 3',5'-di-O-protected-N.sup.4-trimethylsilyl-2'-deoxy-2',2'-difluorocytidi- ne, removing the protecting groups to produce gemcitabine, and, optionally, converting the gemcitabine into a salt. Preferably, the 3' and 5' protecting groups are the same or different, and at least one of the 3' and 5' protecting groups is cinnamoyl, naphthoyl, naphthylmethylcarbonyl, 2-methylbenzylcarbonyl, 4-methylbenzylcarbonyl or 9-fluorenylmethyloxycarbonyl. Also provided are methods for enriching the .beta.-anomer from an anomeric mixture of a 3',5'-di-O-protected-N.sup.4-trimethylsilyl-2'-deoxy-2',2'-difluorocytidi- ne, e.g., a N.sup.4-trimethylsilyl-2'-deoxy-2',2'-difluoro-cytidine-3',5'-diester, e.g., 3',5'-dicinnamoyl-N.sup.4-trimethylsilyl-2'-deoxy-2',2'-difluorocyt- idine, using a slurrying process, and methods for converting the .beta.-anomer-enriched product into gemcitabine or a salt thereof.