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本文研究了十氢十硼酸和它的各种盐类的开笼反应,找到了合成十二氢十硼双二乙基硫醚络合物[B_(10)H_(12)·(Et_2S)_2]的两个新方法。其一,以十氢十硼酸为质子源,水为配位的Lewis碱,打开稳定的B_(10)H_(10)~(2-)笼状骨架,随后用二乙基硫醚处理所得的混合物;其二,以硫酸为质子源,二乙基硫醚为Lewis碱打开B_(10)H_(10)~(2-)的笼状骨架。与文献方法比较,缩短了反应时间,提高了硼的利用率。这些反应与裂解法制备十氢十硼酸双四乙基铵相结合,完成了一条不经过高毒性的十硼烷(14),而由稳定的简单硼氢化合物制备1,2-二碳代-闭-十二硼烷(12)的新的实用路线。
In this paper, the decarboxylation of decahydododecanedioic acid and its various salts has been investigated. The synthesis of [B 10 H 12 (Et 2 S) 2 ] Two new methods. First, a stable B_ (10) H_ (10) ~ (2-) cage was opened by using decahydronadeboronic acid as a proton source and water as Lewis base to treat the resulting Mixture; Second, sulfuric acid as a proton source, diethyl sulfide as Lewis base open B_ (10) H_ (10) ~ (2-) cage-like skeleton. Compared with the literature method, the reaction time is shortened and the boron utilization rate is increased. These reactions, in combination with the bis-tetraethylammonium decahydrate formed by pyrolysis, resulted in the completion of a highly toxic decaborane (14) without the generation of a stable simple borohydride compound, Closed - dodecane (12) of the new practical route.