The present invention provides a method for removing an organic compound in water at a high efficiency by separating an organic compound, particularly such an organic chlorine compound as 1,2-dichloroethane, carbon tetrachloride and chloroform dissolved in water or forming two liquid phases with water from a water phase, by the steps of:(i) charging water containing an organic compound into a first distillation column for conducting distillation or steam distillation to take the organic compound and water out of the top of the first distillation column and to obtain a bottom liquor containing the organic compound at a lower content from the bottom of the first distillation column, and(ii) charging the bottom liquor of the first distillation column into a second distillation column operated at a pressure lower than that in the first distillation column for conducting distillation, preferably flashing under reduced pressure, to take a gas distillate containing a large amount of the organic compound out of the top of the second distillation column and to obtain a bottom liquor containing the organic compound at such a content as to be lower than the organic compound content in the charged liquor from the bottom of the second distillation column.