Abstract: We have developed a high-yield route for the synthesis of [7-'SN]-hypoxanthine in four steps in an overall yield of 81%. This procedure uses ['5N]-sodium nitrite as the I5N source and an inexpensive pyrimidine to provide an economical route to this useful ISN- labeled intermediate. Conversion to [7-'5N]-6-chloropurine followed by enzymatic transglycosylation gives the corresponding ribo-and 2'-deoxyribonucleosides. ...