Abstract: This invention relates to a process for preparing high purity dibromoneopentyl glycol which comprises: (a) charging a vessel with pentaerythritol, a first portion of aqueous HBr and a catalyst; (b) maintaining the liquid contents in the vessel at a temperature from 80.degree. C. to 130.degree. C. for 1 to 3 hours; (c) adding a second portion of aqueous HBr to provide a total HBr to pentaerythritol molar ratio of 1:3 to 1:6; (d) after the foregoing aqueous HBr addition, raising the temperature of the liquid content of the vessel to 120.degree. C. to 180.degree. C.; and (e) sweeping the headspace of the vessel during at least (b), (c) and (d) with an inert gas and removing the sweep gas and any vapors formed during the process from the vessel.