Duroia macrophylla popularly known as "cabeça-de-urubú," "apuruí," or "puruí-grande-da-mata" occurs in the Amazon Forest. Its leaves and branches were collected twice and extracted with dichloromethane and methanol. All extracts were subjected to phytochemical investigation and terpenes and flavonoids were found in all dichloromethane and methanol extracts, respectively. Methanol extracts from both branches (1st collection) and leaves (2nd collection) presented hydrolyzed tannins, yet alkaloids were only detected in the dichloromethane and methanol extracts from branches at the 2nd collection. Phenol compounds were found in both dichloromethane extracts' collections. The action of every extract was assayed against Mycobacterium tuberculosis (RMPr, H37Rv, and INHr strains), showing that the dichloromethane extract from leaves (1st collection) has the major biological activity, with a MIC of 6.25 μg/mL for the INHr strain, 25.0 μg/mL for the RMPr strain, and ≤6.25 μg/mL for the H37Rv strain. The chromatographic fractioning of the dichloromethane extract from leaves (1st collection) yielded the isolation of two triterpenes: oleanolic and ursolic acids, which were identified by NMR analysis and reported for the first time in the Duroia genus.