Selenized glucose is a new product that has recently been used as the starting material for the preparation of selenium-containing catalyst, antibacterial agent, and even heavy metal scavenger. It has potentially important market prospects and commercial value. The chemical can be synthesized by the selenization reaction of glucose with NaHSe, which is generated in situ via the reduction of selenium powder with NaBH4. In this work, we found that oxygen should be strictly avoided during the synthetic reactions and ethanol was the preferable solvent for obtaining the product in stable powder forms. On the basis of these findings, a production line was built to synthesize selenized glucose in kilogram-scale for the first time.