Abstract Chemical investigation of the leave and stem of Pholidota chinensis Lindl has resulted in the isolation and characterization of three new stilbenoids. Their structures were established on the basis of spectroscopic evidence. A series of spin‐labeled stilbene derivatives were synthesized. All of the new compounds were tested for cytotoxicity, and the results revealed that most of the spin‐labeled stilbene derivatives showed superior cytotoxicity in vitro.