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以二-二苯基膦二茂铁二氯化钯(PdCl2(dppf))为催化剂,9,10-二溴蒽和α-萘硼酸为原料,采用Suzuki偶联法合成蓝色发光材料9,10-二(α-萘基)蒽。考察了反应条件,如催化剂用量、溶剂、碱、反应温度、α-萘硼酸与9,10-二溴蒽比率等对反应收率的影响,得出最佳的反应条件是:甲苯/乙醇/水体系(体积比6/1/2);α-萘硼酸与9,10-二溴蒽的物质的量比为3;催化剂量占卤代芳烃的0.5mol%;以碳酸钾为碱,反应7h,收率达到98%,结果远远好于常用的四-三苯基膦钯(Pd(PPh3)4)催化剂。产品经重结晶纯化后,纯度达99%以上,可直接用于OLED器件。
The blue luminescent material 9 was synthesized by the Suzuki coupling method using 9,10-dibromoanthracene and α-naphthaleneboronic acid as the catalyst with bis (diphenylphosphino) ferrocenepalladium dichloride (PdCl2 (dppf)) as the catalyst, 10-bis (α-naphthyl) anthracene. The effects of reaction conditions, such as the amount of catalyst, solvent, base, reaction temperature, the ratio of α-naphthaleneboronic acid and 9,10-dibromoanthracene on the yield of the reaction, were investigated. The best reaction conditions were: toluene / ethanol / Water system (6/1/2 by volume); the amount ratio of α-naphthalene boronic acid to 9,10-dibromoanthracene is 3; the amount of catalyst accounts for 0.5 mol% of the halogenated aromatic hydrocarbon; 7h, the yield reached 98%, the result is far better than the commonly used tetrakis triphenylphosphine palladium (Pd (PPh3) 4) catalyst. After purification by recrystallization, the purity of more than 99%, can be directly used in OLED devices.