Purification Methods
Purify diamantane by repeated crystallisation from MeOH or pentane. Alternatively purify it by dissolving it in CH2Cl2, washing with 5% aqueous NaOH and water, and drying (MgSO4). The solution is filtered, concentrated to a small volume, an equal weight of alumina is added, and the solvent evaporated. The residue is placed on an activated alumina column (ca 4 x weight of diamantane) and eluted with pet ether (b 40-60o). Eight sublimations and twenty zone refining experiments gave material m 251o of 99.99% purity by differential analysis [Gund et al. Tetrahedron Lett 3877 1970, Courtney et al. J Chem Soc Perkin Trans I 2691 1972]. [For spectra see Cupas et al. J Am Chem Soc 87 919 1965.]
