Abstract: An improved process for azeotropic distillation of chloral to anhydrous chloral containing as little as 0.1% water. An azeotropic mixture is used which contains chloral in at least a 1.4:1 ratio with the concentration (% of weight) of a azeotropic agent (preferably ethylene dichloride). The feed stream may contain other components, but will contain at least 60% chloral and less than 40% water. Preferably, the feed stream is substantially free of components other than choral and water. Water is removed from the overhead product of the azeotropic and EDC separation distillations periodically or continuously throughout the process. The azeotropic agent is preferably separated from the anhydrous chloral product. This separation may be performed in the azeotropic distillation column or in a separate distillation column.