Investigation of the MeOH extracts of Sargentia greggii (Rutaceae) led to the isolation of two known flavones, zapotin and 5,6,2''-trimethoxyflavone, and a new flavone, 5,6,2'',3'',4'',6''-hexamethoxyflavone (1), whose structure was established by spectral data and confirmed by total synthesis. In addition, two known coumarins, 3-(.alpha.,.alpha.-dimethylallyl) herniarin and seselin, and a new coumarin, O-geranylosthenol (3), have been isolated from this plant. The structure of 3 was deduced from spectral data. Although the crude extracts displayed KB activity, none of the crystalline compounds were significantly active.