Simple SummarySyrup, a concentrated solution of sugar, is widely used as a sweetener for beverages, foods, and medicines. Palmyra palm syrup is a popular product in Asian countries. Palmyra palm syrup not only provides sweetness to products but also improves food color, aroma, and taste. Palm syrup processing is simple: heating to evaporate water until the total soluble solid reaches 70° Bx. Traditional palmyra palm syrup processing is quick, simple, and low cost and does not require a machine. The disadvantages of palmyra palm syrup are its sensory properties such as dark color, lack of transparency, and it garners less interest than other syrups. Improving the quality of palmyra palm syrup requires increasing the syrup concentration under vacuum condition or using a membrane filter, or both. Palmyra palm syrup prepared by a thermal process had smaller L*, b* values, and larger a* values than that prepared by an ultrafiltration process. Palmyra palm syrup contained 10 vitamins, the most abundant being vitamin E. Overall, 38 volatile compounds were found and classified into six groups in the order of alcohols > acids > ketones > sulfurs > pyrazines > phenols and aldehyde. Volatile compounds depended on concentration, temperature, and ultrafiltration process. Protein content decreased because of participation in the Maillard reaction and increased 5-hydroxymethylfurfural (HMF) and total phenolic content. The HMF content was very low (0.02–14.95 mg/100 g). This study established that ultrafiltration pretreatment of palmyra palm syrup generated a good appearance and reduced the HMF content, however, it negatively affected the volatile compounds and physicochemical characteristics.Palmyra palm syrup, produced from Borassus flabellifer flowers’ sap, is rich in nutrients and minerals and has unique flavors. This study evaluated the in vitro antioxidant activity, physicochemical characteristics, and Maillard reaction products of palmyra palm syrup prepared by thermal and ultrafiltration processes. Palmyra palm syrup prepared by a thermal process had smaller L*, b* values, and larger a* values than that prepared by an ultrafiltration process. Palmyra palm syrup contained 10 vitamins, the most abundant being vitamin E. Overall, 38 volatile compounds were found and classified into six groups in the order of alcohols > acids > ketones > sulfurs > pyrazines > phenols and aldehyde. Volatile compounds depended on concentration, temperature, and ultrafiltration process. Protein content decreased because of participation in the Maillard reaction and increased 5-hydroxymethylfurfural (HMF) and total phenolic content. The HMF content was very low (0.02–14.95 mg/100 g). The radical scavenging activity of 2,2-diphenyl-1-1 picrylhydrazyl and 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulphonic acid) in palmyra palm syrup with thermal process was higher than with ultrafiltration. This study established that ultrafiltration pretreatment of palmyra palm syrup generated a good appearance and reduced the HMF content, however, it negatively affected the volatile compounds and physicochemical characteristics.