| 第 51 卷第 4 期 |  | Vol. 51 No. 4 | | 2021 年 8 月 | Aug 2021 |
|
所屬欄目：功能材料
OLED中間體9-苯基-9-芴醇的合成 |
| 趙素娟，紀春鵬，曲業(yè)芳，谷金儒，蔡洪濤
（中唯煉焦技術(shù)國家工程研究中心有限責任公司，遼寧 鞍山 114000） |
| 摘 要：溴苯的四氫呋喃溶液與鎂粉反應，生成格氏試劑，再與芴酮反應，制備出高純度的OLED中間體9-苯基-9-芴醇，并對反應條件進(jìn)行了優(yōu)化。優(yōu)化條件為：n（溴苯）∶n（鎂粉）∶n（芴酮）=1.3∶1.3∶1.0，反應溫度50~60 ℃。優(yōu)化條件下產(chǎn)品收率達82.5%，純度高于99.5%。產(chǎn)品結構經(jīng)過(guò)IR、MS和1H NMR確認。 |
| 關(guān)鍵詞：溴苯；鎂粉；THF；芴酮；格式試劑 |
| 中圖分類(lèi)號：TQ25 文獻標識碼：A 文章編號：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 |
|
作者簡(jiǎn)介：趙素娟（1979—），女，遼寧鞍山人，高級工程師，碩士，主要從事精細化工。
|
收稿日期：2021-01-12
|
|