Ouratea polygyna is a endemic specie in Brazil. There are no reports phytochemical and biological studies of this specie. The plant material was collected in the Botanical Garden of Rio de Janeiro in September 2018, by the student M. R. da Silva, and Dr. Marcelo da Costa Souza, IB-UFRRJ. The plant material was dried at room temperature and leaves separated from branches to be ground. The extract from the leaves was prepared by maceration with methanol to obtaining about 200 g of crude extract (OPFM). A yellow precipitate was formed in the bottom of the pot. It was separed and washed with dichloromethane to remove a darker coloration, 3 g of solid material was obtained (OPFMP). 1 g of OPFMP was submitted to Sephadex LH-20 Column using a mixture of dichloro-methanol (20:80), increasing the polarity with methanol. About 40 fractions were collected according to similarity by TLC. This procedure was repeated a few times so that material could accumulate. Similar fractions were later collected and analyzed with 1H and 13C NMR spectra to identify components even in mixture. From the fractions 12-13, 17, and 36-40 were identified robustaflavone, 2'-8'' biapigenin and amentoflavone, respectively. The structures of the biflavones were proposed by 1H and 13C NMR spectral data analysis including 1D and 2D experiments, and mass spectra analyses. The liquid part of the extract was submitted to partition with organic solvents and the fraction obtained with ethyl acetate (OPFA is being analyzed and some glucopyranoside derivative are being identified, witch structures are similar to those isolated from Ouratea semiserrata (Ochnaceae), DOI: 10.1002/pca.656.