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J. Chem. Soc., Dalton Trans., 13, p. 2624

DOI: 10.1039/b200930g

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A convenient cyanide-free “one-pot” synthesis of nido-Me3N-7-CB10H12 and nido-7-CB10H13−

Journal article published in 2002 by Andrei S. Batsanov, Mark A. Fox ORCID, Andrés E. Goeta, Judith A. K. Howard, Andrew K. Hughes, John M. Malget
This paper was not found in any repository, but could be made available legally by the author.
This paper was not found in any repository, but could be made available legally by the author.

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Abstract

Reaction of nido-(BuH2N)-Bu-t-7-CB10H12 with Na2CO3 and (MeO)(2)SO2 in THF results in mono-methylation to give nido-(BuMeHN)-Bu-t-7-CB10H12, whilst prolonged reaction at elevated temperatures results in a quantitative yield of the trimethyl derivative nido-Me3N-7-CB10H12, as a result of metathesis of the tert-butyl group. The B-11 NMR spectrum of nido-(BuMeHN)-Bu-t-7-CB10H12 is explored as a function of pH, demonstrating exchange with nido-(BuMeN)-Bu-t-7-CB10H12-. Reaction of B10H14 with CyNC gives nido-CyH2N-7-CB10H12, which is methylated by Na2CO3 and (MeO) 2SO(2) in THF to give nido-CyMe2N-7-CB10H12. Deprotonation of nido-Me3N-7-CB10H12 and nido-CyMe2N-7-CB10H12 yields Na[nido-Me3N-7-CB10H11] and Na[nido-CyMe2N-7-CB10H11] respectively. Both trialkyl( amino) carboranes can be converted to Na[nido-CB10H13], itself a precursor to the poorly coordinating anion closo-CB11H12-. The molecular structures of nido-(BuMeHN)-Bu-t-7-CB10H12 and nido-CyMe2N-7-CB10H12, determined by single crystal X-ray diffraction, are reported.