2,7-二溴-9-亚(β-萘胺)基芴的合成  

Synthesis of N-(2,7-Dibromo-9-fluorenylidene)-β-naphthylamine

作　　者：李奋强[1] 边建红[1] 张鑫[1] 郭建平[1] 张昭[1] 

机构地区：[1]山西大学化学化工学院,山西太原030006

出　　处：《精细化工》2008年第5期518-520,共3页Fine Chemicals

基　　金：山西省自然科学基金(2006011014)~~

摘　　要：以芴为原料,通过空气氧化、水中溴代再与β-萘胺缩合,合成了2,7-二溴-9-亚(β-萘胺)基芴,较佳合成反应条件是:以四氢呋喃为溶剂,空气为氧化剂,n(芴):n(氢氧化钾)=1:2,室温反应6h,得芴酮,产率95.6%,再以芴酮为原料,水为溶剂,n(芴酮):n(溴)=1:2.5,回流反应10h,得2,7-二溴芴酮,然后以四氢呋喃为溶剂,冰乙酸为催化剂,n(2,7-二溴芴酮):n(β-萘胺)=1:1.3,回流反应12h,得2,7-二溴-9-亚(β-萘胺)基芴,产率为87.2%,所得产物的结构经IR、1HNMR、UV-Vis、MS和X射线单晶表征。An important intermediate N- （ 2,7-dibromo-9-fluorenylidene ） -β-naphthylamine which can be used in fine chemicals was prepared from the starting material fluorene through oxidation by air, bromination in water and condensation with β-naphthylamine. The prefenrred reaction conditions are as follows. With THF as solvent, air as oxidant, n （fluorene） ： n （ potassium hydroxide） = 1 ： 2, reacting at room temperature for 6 h, the yield of fluorenone is 95.6%. Sequentially, with water as solvent, n （fluorenone） ：n （bromine） = 1：2. 5 and refluxing for 10 h, then with THF as solvent, acetic acid as catalyst, n （2,7-dibromofluorenone） ： n （β-naphthylamine） = 1 ： 1.3 and refluxing for 12 h, the yield of N- （2,7-dibromo-9-fluorenylidene） -β-naphthylamine is 87.2%. Their structures were characterized by IR, ^1HNMR, UV-Vis, MS and single crystal X-ray.

关 键 词：芴类化合物 亚胺 精细化工中间体 

分 类 号：TQ241.54[化学工程—有机化工]