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)

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:Synthesis by Microwave Irradiation, Crystal Structure and Spectral Properties

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 2-ethoxyethanol 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.