Abstract: To develop the non-invasiveand diagnostic agents for Alzheimer’s disease (AD), ⁹⁹Tc^m(CO)₃⁺-L(L: (E)-2-(4-((4-(dimethylamino)phenyl)diazenyl)phenylamino)acetic acid, adiphenyldiazene derivative) was prepared，radiochemical purity was above 95%. Initialautoradiography results suggested that ⁹⁹Tc^m(CO)₃⁺-Lshowed selective binding to the Aβ plaque-like structures in the brain section from theAD transgenic mice (Tg C57, APP, PS1 12-month-old), further, ⁹⁹Tc^m(CO)₃⁺-Lshowed the same binding sites with fluorescence stained by Re(CO)₃⁺-L.Biodistribution of ⁹⁹Tc^m(CO)₃⁺-L innormal mice demonstrated low uptake in brain (5 min: （0.52 ±0.11)% ID/g）whilst slow clearance from the brain tissues at 120 min post-injection (0.28 ± 0.04)%ID/g. The corresponding Re analogue was alsosynthesized, and the nature of its lowest electronically excited state wasdetermined by studies of the UV-vis absorption and fluorescence emissionproperties at room temperature. In addition, the fluorescent staining of the Re-complexwas performed in comparison to Thioflavin-T and autoradiography results of ⁹⁹Tc^m(CO)₃⁺-L.In conclusion, these results are encouraging for further exploration of ⁹⁹Tc^m(CO)₃⁺-Las a SPECT imaging agent for Aβplaques in the AD brain.