Refers to the procedure of preparation of gemcitabine hydrochloride of formula (i) which consists in: to unlock ') - 1 - (2' - Deoxy 2 ', 2' - difluoro - 3 ',5 '- Di - or - Benzoyl - D - ribofuranosil) - 4 - aminopirimidin - 2 - one with a catalytic amount of an alkylamine as diethylamine,In the presence of methanol or Ethanol and an environment free of water; (b) treating the resulting solution with hydrochloric acid as an antisolvent and acetone, acetonitrile,Tetrahydrofuran or isopropanol, is a Preferred Solvent isopropanol; (c) to recover the resulting Solid gemcitabine hydrochloride
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