This invention relates to a method for separating organic compounds, particularly lower aliphatic alcohols from fermentation fluids. This is accomplished by the use of a two-step extraction process whereby said lower aliphatic alcohols are selectively extracted from said fermentation fluids by a first solvent. The fermentation fluids from which the lower aliphatic alcohols have been extracted contain some of this first solvent. Therefore, a second solvent, which substantially differs from the first solvent in polarity is employed to extract the residual amounts of first solvent from said fermentation fluids. Then, the fermentation fluids, thus purified, can be returned to the fermentation process without the danger of toxic influences on the fermentation by the presence of said first solvent.