Abstract 5'-Chloro-5'-deoxy-2', 3'-O-isopropylideneadenosine reacts with disodium salts of L- homocysteine, L-cysteine or 3-mercaptopropanoic acid in liquid ammonia to afford 2', 3'-O- isopropylidene derivatives which are easily desalted by chromatography on octadecyl-silica column. On acid treatment, the high purity preparations of S-adenosyl-L-homocysteine, S- adenosyl-L-cysteine, and 5'-carboxyethylthio-5'-deoxyadenosine are obtained in ...