A New Synthetic Route to Boron-10 Enriched Pentaborane(9) from Boric Acid and Its Conversion to anti-10B18H22
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Date
2002
Authors
Hosmane, N.S.
Adams, L.A.
Wang, J.
Vyakaranam, K.
Rana, G.
Hosmane, S.N.
Spielvogel, B.F.
Eklund, J.E.
Journal Title
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Volume Title
Publisher
ACS
Abstract
Boron-10 enriched boric acid, H310BO3, was converted to the corresponding sodium borohydride, Na10BH4, in essentially quantitative yields, by using slightly modified literature methods involving the formation of butyl borate, (n-OBu)310B, first and then reacting it with NaH in mineral oil. The oxidation reaction of Na10BH4 with I2 in diglyme and subsequent addition/purification in dioxane gave Na[10B3H8]0.3(C4H8O2) that reacted further with NiCl2 in either anhydrous benzene or heavy mineral oil at 110 °C to produce the corresponding 10B5H9 as the first isolated 10B-enriched liquid boron hydride in a laboratory environment. Treatment of this 10B5H9 with NaH or t-BuLi in 2:1 molar ratio underwent a cage expansion reaction to produce the [M]10B9H14 that undergoes a redox reaction in situ with anhydrous NiCl2 in n-hexane to yield the corresponding fused cage anti-10B18H22 as the only solid borane product in 42% yield, thus establishing new synthetic routes for the preparation of 10B-enriched polyhedral boranes.
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Keywords
Research Subject Categories::NATURAL SCIENCES::Chemistry::Inorganic chemistry::Coordination chemistry
Citation
Adams, L., Hosmane, S. N., Eklund, J. E., Wang, J., & Hosmane, N. S. (2002). A New Synthetic Route to Boron-10 Enriched Pentaborane (9) from Boric Acid and Its Conversion to anti-10B18H22. Journal of the American Chemical Society, 124(25), 7292-7293.