PURPOSE: To prepare highly pure methylchloroform useful as a degreasing agent for metal or a solvent for the treatment of fibers, by adding morpholine to an acid- containing methylchlroform and thereafter separating the precipitate, thereby removing trace of the acid component in high efficiency.

CONSTITUTION: Highly pure methylchloroform is prepared from an acid-containing methylchlorofrom, by mixing the crude methylchloroform with morpholine, and leaving the mixture to stand to separate the precipitate or distilling the mixture. Separation is preferably carried out by distillation to eliminate the problems of deposition of crystal or inactive gel, which frequently occur in the case of leaving the mixture to stand. The amount of morpholine is determined according to the acid content in methylchloroform.