第 51 卷第 4 期 Vol. 51 No. 4 2021 年 8 月 Aug 2021

所属栏目：功能材料 OLED中间体9-苯基-9-芴醇的合成

赵素娟，纪春鹏，曲业芳，谷金儒，蔡洪涛 （中唯炼焦技术国家工程研究中心有限责任公司，辽宁 鞍山 114000）

摘　要：溴苯的四氢呋喃溶液与镁粉反应，生成格氏试剂，再与芴酮反应，制备出高纯度的OLED中间体9-苯基-9-芴醇，并对反应条件进行了优化。优化条件为：n（溴苯）∶n（镁粉）∶n（芴酮）=1.3∶1.3∶1.0，反应温度50~60 ℃。优化条件下产品收率达82.5%，纯度高于99.5%。产品结构经过IR、MS和1H NMR确认。

关键词：溴苯；镁粉；THF；芴酮；格式试剂

中图分类号：TQ25　　文献标识码：A　　文章编号：1009-9212（2021）04-0045-03

Study on Synthesis of 9-Phenyl-9-fluorenol as Intermediate of OLED

ZHAO Su-Juan, JI Chun-peng, QU Ye-fang, GU Jin-ru, CAI Hong-tao (Zhongwei National Engineering Research Center for Coking Technology Co., Ltd., Anshan 114000, China)

Abstract：A high purity OLED intermediate 9-phenyl-9-fluorenol was prepared by the reaction of THF solution of bromobenzene with magnesium powder to form a Grignard reagent and fluorenone. The reaction conditions were optimized, the optimum conditions were as follows: n(bromobenzene)∶n(magnesium powder)∶n(fluorenone)=1.3∶1.3∶1.0, reaction temperature controlled at 55~60 ℃, product yield 82.5%, purity higher than 99.5%. The structure of the product was confirmed by IR, MS and 1H NMR.

Key words：bromobenzene; magnesium powder; THF; fluorenone; Grignard reagent

作者简介：赵素娟（1979—），女，辽宁鞍山人，高级工程师，硕士，主要从事精细化工。

收稿日期：2021-01-12