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This study describes a single step conjugation of Glycylglycine (GlyGly) which is a small peptide, with [18F]FDG via oxime formation. Amiooxy-functionalization of GlyGly (AO-GlyGly) was accomplished through the reaction of Boc-aminooxy succinimide ester. Conjugation reaction was performed at 100 °C for 30 min in a vial containing AO-GlyGly and [18F]FDG solution. The radiolabeled product ([18F]FDG-GlyGly) was obtained with 98.65 ± 0.35% yield without any purification step which makes this method more attractive for 18F radiolabeling. The present study is concluded with an in vivo pilot animal PET study to assess biodistribution and kinetics of chemoselectively [18F]FDG tagged GlyGly in vivo. [ABSTRACT FROM AUTHOR]