Cornus fruits are widely known for possessing anticancer, anti-inflammatory, antioxidant, anti-microbial and hypoglycemic effects. The aim of the study was the detection and isolation of biosynthetic precursors of compounds found in the unripe fruits and the assessment of the antioxidant activity and the ALR2/ALR1 inhibitory activity of their extracts. The LC-DAD-MS (ESI+) analysis revealed the presence of 3-ferulic-3′-ellagic-difuranoside, scandoside methyl ester, and swertiamarin in the Et2O fraction, and cornuside II in the EtOAc fraction. All compounds were found for the first time in C. mas L. Our investigation of the Et2O and EtOAc fractions resulted in the isolation of trans-ferulic acid, gallic acid, methyl gallate, protocatechuic acid, methyl caffeate, trans-p-coumaric acid, caffeic acid, quercetin 3-O-β-D-glucuronide-6′′-methyl ester, 1,2,3,6-tetra-O-galloyl-β-D-glucose, dimethyl malate, quercetin 3-O-β-D-glucuronide, 1,2,3-tri-O-galloyl-β-D-glucose, 1,2,6-tri-O-galloyl-β-D-glucose, 1,2,3,4,6-penta-O-galloyl-β-D-glucose, and 1,2,4,6-tetra-O-galloyl-β-D-glucose. EtOAc extract exhibited the highest scavenging activity determined as EC50 = 0.35 ± 0.01 with the DPPH• assay due to presence of gallotannins while the Et2O had strong antioxidant activity with an IC50 = 0.13 ± 0.01 with the chemiluminescence assay.