三甲基硅基肼的合成

摘要

Using anhydrous hydrazine and trimethyl chlorosilane as raw materials,1,2-bis(trimethylsilyl) hydrazine was synthesized with the yield of 83％.Then through activation of butyllithium,tris(trimethylsilyl) hydrazine were synthesized with the total yield of 75％.Further through solvothermal reaction of lithium-tris(trimethylsilyl)hydrazine and trimethyl chlorosilane,tetra(trimethylsilyl) hydrazine were synthesized with the total yield of 34％.Their structures were characterized by means of NMR,IR,MS and elemental analysis.The self-condensation reaction of mono (trimethylsilyl) hydrazine and rearrangement reaction of bis(trimethylsilyl) hydrazine induced by heat action were analyzed.Results show that these reactions are caused by the inter-and intra-mo-lecular migration of trimethylsilyl group on hydrazine,and isomerization of bis(trimethylsilyl) hydrazine could occur obove 75 ℃.%以无水肼和三甲基氯硅烷为原料,合成了1,2-二(三甲基硅基)肼,收率83％;再经丁基锂活化合成了三(三甲基硅基)肼,总收率75％;进一步通过三(三甲基硅基)肼锂和三甲基氯硅烷的溶剂热反应合成了四(三甲基硅基)肼,总收率34％.通过核磁、红外、质谱和元素分析对上述产物进行了表征.分析了单(三甲基硅基)肼的自缩合反应和双(三甲基硅基)肼在热作用下的重排反应,结果表明,这些反应都是由三甲基硅基在肼基上的分子间和分子内迁移引起的,并且发现75℃以上双(三甲基硅基)就能发生异构体间的转化与平衡.