OLED中间体9-苯基-9-芴醇的合成

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

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^(1)H NMR确认。

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 and1 H NMR.