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以四价铂化合物,即六水合氯铂酸(H2PtCl6·6H2O)和2-苯基吡啶为原料,在微波辐射条件下高产率合成了单环铂金属配合物[(ppy)Pt(Ⅱ)(Hppy)Cl].研究发现,反应分两步进行,首先,六水合氯铂酸和2-苯基吡啶在水:乙二醇单乙醚体积比1:3的混合溶剂中,微波辐射回流反应15min,生成四价铂(Ⅳ)中间产物[(ppy)2Pt(Ⅳ)Cl2];然后,(ppy)2Pt(Ⅳ)Cl2和过量的碳酸钠在微波辐射下反应5min,四价铂被还原成二价铂,得到单环铂金属配合物[(ppy)Pt(Ⅱ)(Hppy)Cl].反应总收率(以H2PtCl6·6H2O计)达到62.1%.采用核磁、质谱、元素分析和单晶X-衍射等仪器对单环金属铂配合物的化学结构、晶体结构和光谱特征进行了表征.
The monocyclic platinum metal complex [(ppy) Pt (Ⅱ) (Ppy) 2 (Ppy) 2 was synthesized by the high yield of tetravalent platinum compounds, namely, H2PtCl6 · 6H2O and 2-phenylpyridine Hppy) Cl] .The study found that the reaction was carried out in two steps, first of all, chloroplatinic acid hexachloride and 2-phenylpyridine in water: ethylene glycol monoethyl ether volume ratio of 1: 3 mixed solvent, microwave radiation reflux reaction 15min (Ppy) 2Pt (Ⅳ) Cl2]; then the reaction of (ppy) 2Pt (Ⅳ) Cl2 and excess sodium carbonate under microwave irradiation for 5 min, the tetravalent platinum is reduced to form a (Pt (Ⅱ) (Hppy) Cl]). The total yield of the reaction (calculated as H2PtCl6 · 6H2O) reached 62.1% .Using NMR, MS, elemental analysis and single crystal X - diffraction and other instruments on the monocyclic metal complexes of platinum chemical structure, crystal structure and spectral characteristics were characterized.