The present invention provides a method for the preparation of 5-azacytidine, wherein 5-azacytidine is represented by the structure: ##STR00001## The method involves the silylation of 5-azacytosine, followed by the coupling of silylated 5-azacytosine to a protected .beta.-D-ribofuranose derivative. The coupling reaction is catalyzed by trimethylsilyl trifluoromethanesulfonate (TMS-Triflate).

 
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