Abstract
Reported is an improved synthesis of essential starting compounds for the development of tricarbollide and metallatricarbollide chemistry. Evaporation of a solution of Na+[5,6-C2B8H11]− (1−) in neat ButNC, followed by acidification, led to the isolation of 7-(ButH2N)-nido-7,8,9-C3B8H10 (2a) in a 90% yield. This was converted into the 7-(H3N)-nido-7,8,9-C3B8H10 (2b) derivative via reaction with AlCl3 in refluxing benzene (yield 77%). Methylation of 2b with Me2SO4 in an alkaline solution gave the 7-(Me3N)-nido-7,8,9-C3B8H10 (2c) derivative in essentially quantitative yield. The reaction of 2c with sodium in liquid ammonia resulted in the formation of highly pure compounds 7-(Me2HN)-nido-7,8,9-C3B8H10 (2d) (yield 71%) and nido-7,8,9-C3B8H12 (3) (yield 19%).
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