双室聚丙烯低温反应瓶的设计制造及在硅芴合成中的应用

设计制造了瓶底有一大一小2个室的聚丙烯（PP）塑料反应瓶，将其用于活泼的金属有机反应中硅芴的合成。 首先将制备的2，2′-二锂基联苯（2）转移到小室中，然后将SiCl4溶液注入大室内，再将反应瓶倾斜，使得化合物2的溶液分次进入大室进行反应，保证反应在SiCl4充分过量条件下进行，可大大降低螺硅芴（4）副反应产物的生成，使9,9-苯基硅芴的产率由20%提高至35%~40%，SiCl4的用量降至4倍摩尔量，从而也降低了产物后处理中柱分离的处理量。

Fabrication of Multiple-tank Polypropylene Bottles and Its Application in Synthesizing Silafluorene

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.