A.S. Batsanov
A convenient cyanide-free 'one-pot' synthesis of nido-Me₃N-7-CB₁₀H₁₂ and nido-7-CB₁₀H₁₃
Batsanov, A.S.; Fox, M.A.; Goeta, A.E.; Howard, J.A.K.; Hughes, A.K.; Malget, J.M.
Authors
M.A. Fox
A.E. Goeta
J.A.K. Howard
A.K. Hughes
J.M. Malget
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.
Citation
Batsanov, A., Fox, M., Goeta, A., Howard, J., Hughes, A., & Malget, J. (2002). A convenient cyanide-free 'one-pot' synthesis of nido-Me₃N-7-CB₁₀H₁₂ and nido-7-CB₁₀H₁₃. Dalton Transactions, 2624-2631. https://doi.org/10.1039/b200930g
Journal Article Type | Article |
---|---|
Publication Date | May 1, 2002 |
Deposit Date | May 15, 2007 |
Journal | Dalton Transactions |
Print ISSN | 1477-9226 |
Publisher | Royal Society of Chemistry |
Peer Reviewed | Peer Reviewed |
Issue | 13 |
Pages | 2624-2631 |
DOI | https://doi.org/10.1039/b200930g |
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