在碱性条件下,以铱的氯桥二聚体(dfppy)2Ir(μ-Cl2)Ir(dfppy)2和乙酰丙酮反应合成出高效磷光材料二[2-(2,4-二氟苯基)吡啶-C2,N'](乙酰丙酮)合铱(III)(Ir(dfppy)2(acac))。用核磁共振谱(1H NMR、13C NMR)、红外光谱和单晶 X 射线衍射等表征手段确定了分子结构,用高效液相色谱法测定了纯度,用光致发光光谱测试了光物理性能。结果表明,合成的配合物组成及结构与实际一致,Ir(dfppy)2(acac)为电中性八面体配合物,Ir-O、Ir-C、Ir-N键的平均长度分别为0.2160(14)、0.1998(11)、0.2030(15) nm,在484 nm处出现了较强的蓝光发射。方法的合成产率大于90%,纯度99.70%,适于批量制备。
A new chemical technique was developed for batch synthesis of bis(2,4-difluorophenyl-pyridine-C2,N')(acetylacetonato)iridium(III), an organometallic light-emitting molecule for OLED. The process involves the reaction of a chloride-bridged dimer with acetylactone to produce the desired compound in a 10~20 gram batch scale. The yield was more than 90%, and the purity was determined by HPLC to be 99.70%. The chemical structure of the product was verified by NMR (1H and 13C) and FT-IR along with single crystal X-ray diffraction. The structural data show that Ir(dfppy)2(acac) is an electrically neutral octahedral complex. The average bond lengths of Ir-O, Ir-C and Ir-N are 0.2160(14), 0.1998(11) and 0.2030(15) nm, respectively. The iridium(Ⅲ) complex develops a strong emission band at 484 nm.
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