四川师范大学学报(自然科学版)
四川師範大學學報(自然科學版)
사천사범대학학보(자연과학판)
JOURNAL OF SICHUAN NORMAL UNIVERSITY(NATURAL SCIENCE)
2010年
6期
816-820
,共5页
骆开均%景凯%谢运%徐玲玲%王建维
駱開均%景凱%謝運%徐玲玲%王建維
락개균%경개%사운%서령령%왕건유
单核铂配合物%微波辐射%晶体结构
單覈鉑配閤物%微波輻射%晶體結構
단핵박배합물%미파복사%정체결구
mononuclear platinum(II) complex%microwave irradiation%crystal structure
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15 min,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5 min,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.
以四價鉑化閤物,即六水閤氯鉑痠(H2PtCl6·6H2O)和2-苯基吡啶為原料,在微波輻射條件下高產率閤成瞭單環鉑金屬配閤物[(ppy)Pt(II)(Hppy)Cl].研究髮現,反應分兩步進行,首先,六水閤氯鉑痠和2-苯基吡啶在水:乙二醇單乙醚體積比1:3的混閤溶劑中,微波輻射迴流反應15 min,生成四價鉑(IV)中間產物[(ppy)2Pt(IV)Cl2];然後,(ppy)2Pt(IV)Cl2和過量的碳痠鈉在微波輻射下反應5 min,四價鉑被還原成二價鉑,得到單環鉑金屬配閤物[(ppy)Pt(II)(Hppy)Cl].反應總收率(以H2PtCl6·6H2O計)達到62.1%.採用覈磁、質譜、元素分析和單晶X-衍射等儀器對單環金屬鉑配閤物的化學結構、晶體結構和光譜特徵進行瞭錶徵.
이사개박화합물,즉륙수합록박산(H2PtCl6·6H2O)화2-분기필정위원료,재미파복사조건하고산솔합성료단배박금속배합물[(ppy)Pt(II)(Hppy)Cl].연구발현,반응분량보진행,수선,륙수합록박산화2-분기필정재수:을이순단을미체적비1:3적혼합용제중,미파복사회류반응15 min,생성사개박(IV)중간산물[(ppy)2Pt(IV)Cl2];연후,(ppy)2Pt(IV)Cl2화과량적탄산납재미파복사하반응5 min,사개박피환원성이개박,득도단배박금속배합물[(ppy)Pt(II)(Hppy)Cl].반응총수솔(이H2PtCl6·6H2O계)체도62.1%.채용핵자、질보、원소분석화단정X-연사등의기대단배금속박배합물적화학결구、정체결구화광보특정진행료표정.
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.