An investigation of the use of KF/alumina for the deboronation of o-carborane is described. The percentage of deboronation of o-carborane in acetonitrile, glyme, and tetrahydrofurn under a variety of reaction conditions has been determined. Complete deboronation is accomplished when wet refluxing acetonitrile is employed as the solvent. High yields of [P(C6H5)(3)CH3][nido-7,8-C2B9H12] have been obtained from the deboronation of o-carborane by the use of KF/alumina in wet acetonitrile.