摘要
以碳酸丙烯酯为溶剂、以N-溴代丁二酰亚胺(NBS)为溴化试剂,进行芴的溴代反应研究,合成了2-溴芴和2,7-二溴芴。通过对反应温度、NBS的用量以及加入方式等的考察,确定合成2-溴芴的最佳反应条件。最佳反应条件为:反应温度23℃、NBS和芴的物质的量比为1.1∶1、NBS分批加入。先将芴和碳酸丙烯酯预热至60℃,使得芴全部溶解,然后降至反应温度,分批加入NBS。2-溴芴和2,7-二溴芴分别以无水乙醇和冰醋酸重结晶,目标产物的液相色谱纯度均可达到99%以上。
The 2-bromofluorene and 2,7-dibromofluorene were synthesized with using propylene carbonate as solvent and N-bromosuccinimide (NBS) as bromination agent. The influence of reaction temperature, ratio of NBS to fluorene and the feeding mode was investigated. The optimal reaction conditions were obtained as follows: the reaction temperature was 23℃, the ratio of NS to fluorene was 1.1:1 and the stage addition was adopted. The fluorene and propylene carbonate was heated to 60℃, made the fluorene dissolve completely, and then made it drop to the reaction temperature, and fed the NBS through the stage addition. The 2-bromofluorene and 2,7-dibromofluorene were recrystallized from ethanol and acetic acid respectively, and the liquid chromatogram purity of objective products could reach over 99%.
出处
《化学与粘合》
CAS
2012年第1期29-31,共3页
Chemistry and Adhesion
基金
哈尔滨市科技局攻关项目(编号:2007AA4CG068)
关键词
NBS
2-溴芴
2
7-二溴芴
溴化
NBS
2-bromofluorene
2,7-dibromofluorene
bromination