Abstract: An improved process of distilling a cyclohexanone-rich overhead stream in a first still from a feed mixture comprising cyclohexanone, phenol and cyclohexanol of the type wherein a cyclohexanone-rich stream is withdrawn as a part of an overheads condensate from the first still and a phenol-rich stream is withdrawn as a part of a reboiled bottom stream from the first still. The improvement includes withdrawing a side stream substantially free of phenol from above the point where the feed mixture is fed to the first column and separating the side stream in a second still into a second cyclohexanone-rich overhead stream and a bottom stream containing cyclohexanone and cyclohexanol. The second cyclohexanone-rich stream may be returned to the first still.