The synthesis and characterization of two novel biscoumarin derivatives (1 and 2) were realized by means of IR, H-1 NMR, HRMS and single crystal X-ray crystallography. The anti- gastrointestinal cancer activity of the two compounds were investigated against four human gastrointestinal cancer cells (GES- 1, SGC- 7901, BGC- 823 and MGC- 803) by MTT assay. It has been found that compound 2 exerted much more potent activity against the four cell lines than compound 1.