Abstract: Four kinds of norcantharidin derivatives are synthesized and the coupling compounds are prepared individually. The compounds are labeled by))~99)Tc~m and the labeling yield is mostly over 90% under the best condition (3.0 mmol/L SnCl2;pH=7～8; reaction temperature, 100 ℃;reaction time, 30 min). Two samples are chosed for biodistribution experiments. The reaults show that the labeled N-animo-5,6-bibromine norcantharidin has a higher uptake in liver and gallbladder, and the labeled DTPA-N-)animo-5,6-bibromine norcantharidin is mainly concentrated in kidney. Both labeled compounds clear quickly in blood.