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SiC14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.
参考文献
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