Simple column chromatography using 10%-moist silica gel enabled efficient removal of organotin residues from geranyl acetate, which was prepared by the acetylation of geraniol with vinyl acetate in the presence of a catalytic amount of a 1,3-dichloro-substituted tetrabutyldistannoxane. The desired acetate contained only 2.4 ppm of organotin residues. In sharp contrast to this, a similar purification method using dry silica as the stationary phase provided acetate containing ca. 5000 ppm of organotin residues.