小中大[求助]六溴代三叠烯制备
本人最近在做一个反应,用到一个底物六溴代的三蝶烯,根据文献来看貌似很简单的一个溴化过程,但是我做的产物,一直非常不纯,感觉只上了三个溴,溴化过程也是按着文献所述来的,有没有大神指导一下,有做过的就更好了
文献描述如下:Triptycene (1.06 g, 4.18 mmol) was dissolved in chloroform (80 mL) in a round-bottom flask. Iron filings (30mg) were added, and the solution was stirred at 25 °C. Bromine (1.35 mL, 26.3 mmol) was added, and the solution was refluxed for 1 h, during which time the initially reddish-brown solution turned reddish-orange. The flask was removed from heat, and chloroform and excess bromine were removed under vacuum. The resulting brown powder was dissolved in chloroform (100 mL) and flushed through a pad of silica using additional chloroform as eluent (100 mL). The filtrate was evaporated to dryness。----《A Triphenylene-Based Triptycene with Large Free Volume Synthesized by Zirconium-Mediated Biphenylation》