Citation:
MO Yueqi, CHANG Xueyi. Fabrication of Multiple-tank Polypropylene Bottles and Its Application in Synthesizing Silafluorene[J]. Chinese Journal of Applied Chemistry,
;2012, 29(7): 852-854.
doi:
10.3724/SP.J.1095.2012.00358
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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.
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