PURPOSE: To obtain anhydrous inositol crystal free from impurity in high yield of crystallization with low heat load in drying process by crystallizing an inositol-containing aqueous solution with an alcohol.

CONSTITUTION: An inositol-containing aqueous solution is crystallized with an alcohol (e.g. usually ethanol) at 0-40°C, filtered by a centrifugal separator, etc., and dried to give pure anhydrous inositol crystal. The amount of the alcohol added is preferably 4-6 volumes based on 1 volume water in the aqueous solution. Before pouring the alcohol, the aqueous solution is treated with active carbon or ion exchange resin alone or both, thermal concentration process of the aqueous solution is added or cooling operation in crystallizing process is provided to give the aimed substance much more effectively.