3-溴螺环[芴-9,9’-氧杂蒽]的合成工艺研究  

Study on Synthesis Process of 3-Bromospiro[fluorene-9,9’-xanthene]

作　　者：李瑞 汪波洋 李国防[1] 申娟娟 刘畅 杨振强[1] LI Rui;WANG Boyang;LI Guofang;SHEN Juanjuan;LIU Chang;YANG Zhenqiang(Henan Academy of Sciences Institute of Chemistry Co.,Ltd.,Zhengzhou 450002,China;Changshuo Technology(Shanghai)Co.,Ltd.,Shanghai 200120,China)

机构地区：[1]河南省科学院化学研究所有限公司,河南郑州450002 [2]昌硕科技(上海)有限公司,上海201200

出　　处：《化工技术与开发》2022年第4期10-12,共3页Technology & Development of Chemical Industry

基　　金：河南省科学院重大聚焦项目(210103001);河南省科学院特聘研究员项目(200503001)。

摘　　要：螺[芴-9,9’-氧杂蒽]衍生物作为蓝光材料或掺杂材料,被广泛应用于有机发光半导体(OLED)器件。本文以二苯醚为起始原料,经仲丁基锂锂化后,与3-溴-9H-芴酮反应得到中间体化合物,在二氯甲烷溶剂中,经对甲基苯磺酸催化闭环反应,合成了3-溴螺环[芴-9,9’-氧杂蒽]。研究表明,当锂化反应温度为-45℃,原料n(二苯醚)∶n(3-溴-9H-芴酮)=1.0∶0.8时,目标化合物的总收率最高达到75%。Spiro[fluorene-9,9’-xanthene] derivatives were widely used in organic light emitting semiconductor(OLED) devices as blue light materials or dopant materials. In this paper, 3-bromospiro[fluorene-9,9’-xanthene] was synthesized applied diphenyl ether as the starting material, then reacted with 3-bromo-9H-fluorenone after being lithiated by sec-butyl lithium, and then via ring closure reaction by p-toluenesulfonic acid catalysis in dichloromethane solvent. Studies results showed that when the lithiation reaction temperature was-45℃,the raw material n(diphenyl ether): n(3-bromo-9H-fluorenone) = 1.0: 0.8, total yield of the target compound reached to 75%.

关 键 词：二苯醚 螺环[芴-9 9’-氧杂蒽] 合成 

分 类 号：O625.153[理学—有机化学]