J. Holub et al., POLYHEDRAL CARBATHIABORANE CHEMISTRY - 10-VERTEX NIDO AND ARACHNO, 11-VERTEX NIDO, AND 8-VERTEX HYPHO FAMILIES OF CARBATHIABORANES, Journal of the Chemical Society. Dalton transactions, (8), 1994, pp. 1317-1323
Treatment of arachno-4-CB8H14 with sulfur and triethylamine in chlorof
orm has produced the new ten-vertex carbathiaborane arachno-6,9-CSB8H1
2, which has been used for the preparation of a series of further carb
athiaborane compounds. Deprotonation with sodium hydride or 1,8-bis(di
methylamino)-naphthalene generates the [arachno-6,9-CSB8H11]- anion. T
hermolysis of the sodium salt of this anion, followed by acidification
, results in comproportionation to give nido-7,9-CSB9H11 and arachno-4
,6-CSB7H11. Alternatively, oxidation by acetone yields the [nido-6,9-C
SB8H9]- anion. Degradation of this latter anion with concentrated hydr
ochloric acid leads to arachno-4,6-CSB7H11. Deprotonation of this neut
ral carbathiaborane with sodium hydride in ether, followed by degradat
ion by aqueous acetone of the [arachno-4,6-CSB7H10]- anion generated i
n situ, gives the [hypho-7,8-CSB6H11]- anion. This has been methylated
by methyl iodide to afford neutral 8-Me-hypho-7,8-CSB611. The unambig
uous cluster constitutions of all compounds isolated have been establi
shed by H-1 and B-11 NMR spectroscopy and mass spectrometry.