关键词: 金属有机化学反应, 多室反应瓶, 聚硅芴

Abstract: In order to improve the yield of synthesizing silafluorene, a plastic multiple-tank reaction bottle was designed and fabricated. It was well-known that the reaction of 4,4′-dibromo-2,2′-diiodobiphenyl(1) with butyllithium formed a key active intermediate 4,4′-dibromo-2,2′-dilithiumbiphenyl(2), which should be kept under low temperature. In our previous work, we added a large excess of SiCl4(20 fold in molar ratio) into the solution of compound 2 to suppress the formation of spirosilafluorene(4). In this contribution, the use of a plastic multiple-tank reaction bottle made it possible to add the solution of compound 2 into SiCl4 because it provides compound 2 with a container in the bottom of the bottle. By leaning the reaction bottle, compound 2 can be transferred into the storage tank or transfer into the reaction tank under low temperature. This new apparatus can improve the yield of the silafluorene from 20% to 35%~40% with a much less SiCl4 feed ratio(4 fold in molar ratio). This plastic multiple-tank reaction bottle might be widely used in the organometallic chemistry.

Key words: organometallic chemistry, multiple-tank plastic reaction bottle, silafluorene.