(1) Background: This study is designed to extract the bioactive compounds from beetroot peel for future use in the food industry. (2) Methods: Spectrophotometry techniques analyzed the effect of conventional solvent extraction on betalains and polyphenolic compounds from beetroot peels. Several treatments by varying for factors (ethanol and citric acid concentration, temperature, and time) were applied to the beetroot peel samples. A Central Composite Design (CCD) has been used to investigate the effect of the extraction parameters on the extraction steps and optimize the betalains and total polyphenols extraction from beetroot. A quadratic model was suggested for all the parameters analyzed and used. (3) Results: The maximum and minimum variables investigated in the experimental plan in the coded form are citric acid concentration (0.10–1.5%), ethanol concentration (10–50%), operating temperature (20–60 °C), and extraction time (15–50 min). The experimental design revealed variation in betalain content ranging from 0.29 to 1.44 mg/g DW, and the yield of polyphenolic varied from 1.64 to 2.74 mg/g DW. The optimized conditions for the maximum recovery of betalains and phenols were citric acid concentration 1.5%, ethanol concentration 50%, temperature 52.52 °C, and extraction time 49.9 min. (4) Conclusions: Overall, it can be noted that the extraction process can be improved by adjusting operating variables in order to maximize the model responses.