Journal
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
Volume 58, Issue 9, Pages 2720-2724Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/anie.201812795
Keywords
alkali metals; boron; nucleophilicity; reaction mechanisms; X-ray diffraction
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Funding
- National Natural Science Foundation of China [U1804253, 21771057]
- Science and Technology Committee of Shanghai [17ZR1402500, 16520721800]
- U.S. National Science Foundation [DMR-1655066]
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A facile synthesis of heavy alkali metal octahydrotriborates (MB3H8; M=K, Rb, and Cs) has been developed. It is simply based on reactions of the pure alkali metals with THFBH3, does not require the use of electron carriers or the addition of other reaction media such as mercury, silica gel, or inert salts as for previous procedures, and delivers the desired products at room temperature in very high yields. However, no reactions were observed when pure Li or Na was used. The reaction mechanisms for the heavy alkali metals were investigated both experimentally and computationally. The low sublimation energies of K, Rb, and Cs were found to be key for initiation of the reactions. The syntheses can be carried out at room temperature because all of the elementary reaction steps have low energy barriers, whereas reactions of LiBH4/NaBH4 with THFBH3 have to be carried out under reflux. The high stability and solubility of KB3H8 were examined, and a crystal structure thereof was obtained for the first time.
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