湖北大学学报(自然科学版)
湖北大學學報(自然科學版)
호북대학학보(자연과학판)
2015年
5期
484-487
,共4页
毕峰%姚骏%齐磊%洪啸%柳利%李法宝
畢峰%姚駿%齊磊%洪嘯%柳利%李法寶
필봉%요준%제뢰%홍소%류리%리법보
芴%亚膦酸二乙酯%发光材料%合成%表征
芴%亞膦痠二乙酯%髮光材料%閤成%錶徵
물%아련산이을지%발광재료%합성%표정
fluorene%diethylphosphate%intermediate%synthesis%characterization
具有刚性结构、高稳定性和发光效率、结构易于修饰的芴基发光材料引起广泛关注.以芴为原料,通过卤代反应获得溴芴后,在钯试剂催化下,与亚膦酸二乙酯进行偶联反应,合成了目标化合物2-芴基膦酸二乙酯.采用核磁共振谱(1H、13C、31P NMR)、傅里叶变换红外光谱(FT-IR)、液质联用飞行时间质谱(LC-MS TOF)等对目标化合物进行结构表征,确证了结构.与传统的合成膦酸酯的方法相比,该法具有收率高、操作简便、反应条件温和等优点.该化合物目前少见报道.①
具有剛性結構、高穩定性和髮光效率、結構易于脩飾的芴基髮光材料引起廣汎關註.以芴為原料,通過滷代反應穫得溴芴後,在鈀試劑催化下,與亞膦痠二乙酯進行偶聯反應,閤成瞭目標化閤物2-芴基膦痠二乙酯.採用覈磁共振譜(1H、13C、31P NMR)、傅裏葉變換紅外光譜(FT-IR)、液質聯用飛行時間質譜(LC-MS TOF)等對目標化閤物進行結構錶徵,確證瞭結構.與傳統的閤成膦痠酯的方法相比,該法具有收率高、操作簡便、反應條件溫和等優點.該化閤物目前少見報道.①
구유강성결구、고은정성화발광효솔、결구역우수식적물기발광재료인기엄범관주.이물위원료,통과서대반응획득추물후,재파시제최화하,여아련산이을지진행우련반응,합성료목표화합물2-물기련산이을지.채용핵자공진보(1H、13C、31P NMR)、부리협변환홍외광보(FT-IR)、액질련용비행시간질보(LC-MS TOF)등대목표화합물진행결구표정,학증료결구.여전통적합성련산지적방법상비,해법구유수솔고、조작간편、반응조건온화등우점.해화합물목전소견보도.①
Fluorene-based luminescent materials have been paid great attention due to their rigid structure,high stability and luminescenc efficiency,as well as easily modified structures.We described the synthesis of the title compound 2- fluorenyl diethyl phosphonate using fluorene as starting material by halogenation and palladium-catalyzed coupling reactions.The structure of the title compound was characterized and confirmed by NMR(1H,13C and 31P),FT-IR and LC-MS TOF spectra.Comparing with traditional methods, this method has advantages of high yield,simplification of operation process and mild reaction condition.As far as we know,the title compound has not more been reported.