摘要
以芴、溴素为原料,三氯甲烷为溶剂,铁粉为催化剂,0℃下合成得到2,7-二溴芴,然后以二甲基亚砜为溶剂,四丁基溴化铵为相转移催化剂,室温下与1-溴辛烷反应得到标题化合物,总收率为53.2%。通过1HNMRI、R和元素分析确证了2,7-二溴芴与标题化合物的结构。与目前常用的3种合成方法相比较,该合成工艺具有反应条件温和,后处理简单,收率较高等优点。
2,7-Dibromofluorene was synthesized with fluorene and bromine as starting materials in chloroform solution in the presence of iron powder as the catalyst at 0℃, followed by reacting with 1-bromooctane in DMSO solution in the presence of tetrabutylammoniumbremide as the phase transfer catalyst at room temperature. The title compound 2,7-dibromo-9,9-dioctylfluorene was prepared with its total yield reaching 53.2% .The structures of 2, 7-dibremofluorene and 2, 7-dibromo-9, 9-dioctylfluorene were determined by 1HNMR, IR and elementary analysis. Compared with three conventional synthetic methods, the present synthesis condition was mild along with a simple after-treatment process leading to high product yield.
出处
《化学试剂》
CAS
CSCD
北大核心
2007年第2期117-118,123,共3页
Chemical Reagents
基金
湖南省自然科学基金资助项目(06JJ200805JJ40019)