The red aqueous beverages of Carapa procera (D.C.) leaf extracts were investigated for their polyphenol contents using HPLC-DAD, HPLC-ESI-MS, and semipreparative HPLC. Polyphenols were extracted, clarified, and concentrated using a multistep process including ultrasound-assisted extraction (UAE), cross-flow microfiltration (CFM), and reverse osmosis (RO). On the basis of analytical and semipreparative chromatographic techniques, 12 phenolic compounds were identified and quantified for the first time: 2 anthocyanins (cyanidin 3-O-glucoside and cyanidin 3-O-rutinoside), 5 phenolic acids (protocatechuic, the three caffeoylquinic isomers, and coumaroylquinic acid), and 5 flavonols (quercetin 3-O-rutinoside, quercetin 3-O-galactoside, quercetin 3-O-glucoside, quercetin aglycone, and kaempferol 3-O-rutinoside). From the concentrated extract, it was possible to recover for anthocyanins (28.4 ± 0.3 µmol L⁻¹ cyanidin equivalents) the two glycosides of cyanidin, for flavonols (1587 ± 3 µmol L⁻¹ quercetin equivalents) the two glycosides of quercetin and kaempferol, and for phenolic acids (3650 ± 10 µmol L⁻¹ gallic acid equivalents) chlorogenic and protocatechuic acids.