单核铂配合物(ppy)Pt(Hppy)Cl的微波合成、晶体结构及其光谱性质(英文)

Mononuclear Platinum(Ⅱ) Complex with 2-phenylpyridine Ligands:Synthesis by Microwave Irradiation,Crystal Structure and Spectral Properties

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.

Mononuclear platinum（Ⅱ） complex with 2-phenylpyridine ligands,（ppy） Pt（Ⅱ）（Hppy） Cl has been synthesized by the reaction of Pt（Ⅳ） compound,H2PtCl6·6H2O,and 2-phenylpyridine under microwave irradiation.Firstly,with reflux during microwave irradiation for 15 min in the 3：1 mixture solvent of 2ethoxyethanol and water,the Pt（Ⅳ） compound,H2PtCl6 ·6H2O reacts with 2-phenylpyridine to form Pt（Ⅳ） complex with the structure of（ppy） 2Pt（Ⅳ） Cl2;then,（ppy） 2Pt（Ⅳ） Cl2 is reduced and dissociated in the presence of excess sodium carbonate（Na2CO3） after microwave irradiation for 5 min into the final title complex with the structure of（ppy） Pt（Ⅱ）（Hppy） Cl.The total yield based on H2PtCl6·6H2O is 62.1%.The title compound has been characterized by 1HNMR,MS-EIS and single-crystal X-ray structure analysis.