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Nucleophilic substitution at the exo polyhedral boron atoms of closo decaborate [B 10 H 10 ] 2-in the presence of carbocations, which were generated in situ from various halocarbons (triphe nylmethyl chloride, 1 bromoadamantan, n butyl bromide), was studied. The reactions carried out in nucleophilic solvents (cyclic ethers and thioethers, N,N disubstituted amides, and car boxylic acids) and in the presence of halocarbons afforded mono and disubstituted compounds with the exo polyhedral B-O and B-S bonds, which contained a molecule of the solvent as substituent. The structures of the compounds synthesized were confirmed by the IR, mass, and 1 H, 11 B, and 13 C NMR spectra.

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