This paper describes the procedures for the facile synthesis of 9,9′-bis(methoxymethyl)fluorene using fluorene as starting material. By hydroxymethylation and etherification reaction, the fluorene can be converted to...This paper describes the procedures for the facile synthesis of 9,9′-bis(methoxymethyl)fluorene using fluorene as starting material. By hydroxymethylation and etherification reaction, the fluorene can be converted to desired products with high yield and purity. The optimum conditions of the synthetic procedures were determined. For hydroxymethylation, the reaction temperature was 13 ℃and the mole ratio of sodium methoxide to paraformaldehyde was 0.26; and for etherification, the reaction temperature was 40 ℃and the reaction time was 15 h. Under the optimum conditions, an overall yield of 580 0 and purity of 99.20 0 were obtained.展开更多
Synthesis of 9,9-bis（buthoxyearbonylethyl） fluorine（C27 H34 04, Mr= 422.54） with butyl acrylate as alkylation reagent and fluorene as starting material has been performed. The crystal structure was measured by usi...Synthesis of 9,9-bis（buthoxyearbonylethyl） fluorine（C27 H34 04, Mr= 422.54） with butyl acrylate as alkylation reagent and fluorene as starting material has been performed. The crystal structure was measured by using the X-ray diffraction method. The crystal belongs to monoclinic, space group P2 （1）/c with parameters as： a=l. 2912（1）nm, b=l. 0974（1）nm, c=1. 7468（1）nm, β=90. 252（2）, V=2. 4752（4）nm^3 , Z=4, Dcacl= 1. 134 g · cm^-3 ,λ=0. 071 073 nm, μ（MoKα） =0. 075mm^-1 , F（000） =912, R=0. 0651 and wR=0. 1475. X-ray analysis reveals that the three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system, weak CH O hydrogen-bonding connects the molecule into centrosymmetric dimmers展开更多
合成了一种具有深的HOMO(-6.15 e V)分子轨道和高三线态能级(T_1,2.82 e V)的新型化合物10-(2-螺-9,9'-氧杂蒽芴基)吩噻嗪(SFXPz)。因其宽的能带结构(E_g,4.22 e V)和深的HOMO能级而有望制备高效蓝色有机电致磷光器件。热重分析和...合成了一种具有深的HOMO(-6.15 e V)分子轨道和高三线态能级(T_1,2.82 e V)的新型化合物10-(2-螺-9,9'-氧杂蒽芴基)吩噻嗪(SFXPz)。因其宽的能带结构(E_g,4.22 e V)和深的HOMO能级而有望制备高效蓝色有机电致磷光器件。热重分析和差热扫描曲线表明,该化合物具有良好的热稳定性(T_d,259℃)和高的形态稳定性(T_g,206℃)。完全相互分离的HOMO和LUMO轨道有利于阻止分子内能量反转。SFXPz的紫外吸收峰分别位于230,260,292和310 nm左右;其荧光光谱两个发射峰分别位于311,324 nm左右。此外,该化合物的分子结构经LC-MS、~1H NMR和^(13)C NMR进行了详细表征。展开更多
As a novel class of spirofluorenes,spirobifluorene(SBF)and spiro[fluo-rene-9,9'-xanthene]derivatives(SFXs)have orthogonal geometric config-uration,spiro-conjugation effect,and rigid steric hindrance,which can be w...As a novel class of spirofluorenes,spirobifluorene(SBF)and spiro[fluo-rene-9,9'-xanthene]derivatives(SFXs)have orthogonal geometric config-uration,spiro-conjugation effect,and rigid steric hindrance,which can be widely used in the fields of synthetic chemistry,materials chemistry and supramolecular chemistry.Due to their facile one-pot synthetic route,and to the variety of molecular designs,SFXs are expected to become new spiro functional materials that replace SBF.In this review,we present the history,development and expansion of SFXs synthesis in one-pot methods,and the advantages and limitations of one-pot synthesis are also dis-cussed.展开更多
文摘This paper describes the procedures for the facile synthesis of 9,9′-bis(methoxymethyl)fluorene using fluorene as starting material. By hydroxymethylation and etherification reaction, the fluorene can be converted to desired products with high yield and purity. The optimum conditions of the synthetic procedures were determined. For hydroxymethylation, the reaction temperature was 13 ℃and the mole ratio of sodium methoxide to paraformaldehyde was 0.26; and for etherification, the reaction temperature was 40 ℃and the reaction time was 15 h. Under the optimum conditions, an overall yield of 580 0 and purity of 99.20 0 were obtained.
基金Foundation of Huangshi Institute of Technology(2008yjz27B)
文摘Synthesis of 9,9-bis（buthoxyearbonylethyl） fluorine（C27 H34 04, Mr= 422.54） with butyl acrylate as alkylation reagent and fluorene as starting material has been performed. The crystal structure was measured by using the X-ray diffraction method. The crystal belongs to monoclinic, space group P2 （1）/c with parameters as： a=l. 2912（1）nm, b=l. 0974（1）nm, c=1. 7468（1）nm, β=90. 252（2）, V=2. 4752（4）nm^3 , Z=4, Dcacl= 1. 134 g · cm^-3 ,λ=0. 071 073 nm, μ（MoKα） =0. 075mm^-1 , F（000） =912, R=0. 0651 and wR=0. 1475. X-ray analysis reveals that the three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system, weak CH O hydrogen-bonding connects the molecule into centrosymmetric dimmers
文摘合成了一种具有深的HOMO(-6.15 e V)分子轨道和高三线态能级(T_1,2.82 e V)的新型化合物10-(2-螺-9,9'-氧杂蒽芴基)吩噻嗪(SFXPz)。因其宽的能带结构(E_g,4.22 e V)和深的HOMO能级而有望制备高效蓝色有机电致磷光器件。热重分析和差热扫描曲线表明,该化合物具有良好的热稳定性(T_d,259℃)和高的形态稳定性(T_g,206℃)。完全相互分离的HOMO和LUMO轨道有利于阻止分子内能量反转。SFXPz的紫外吸收峰分别位于230,260,292和310 nm左右;其荧光光谱两个发射峰分别位于311,324 nm左右。此外,该化合物的分子结构经LC-MS、~1H NMR和^(13)C NMR进行了详细表征。
基金the National Natural Science Foundation of China(21774061,2207112 and 61935017)Natural Science Foundation major research program integration project(Grant Number 91833306)+1 种基金Six Peak Talents Foundation of Jiangsu Province(XCLCXTD-009)Open Project from State Key Labor-atory of Supramolecular Structure and Materials at Jilin University(No.sklssm202014).
文摘As a novel class of spirofluorenes,spirobifluorene(SBF)and spiro[fluo-rene-9,9'-xanthene]derivatives(SFXs)have orthogonal geometric config-uration,spiro-conjugation effect,and rigid steric hindrance,which can be widely used in the fields of synthetic chemistry,materials chemistry and supramolecular chemistry.Due to their facile one-pot synthetic route,and to the variety of molecular designs,SFXs are expected to become new spiro functional materials that replace SBF.In this review,we present the history,development and expansion of SFXs synthesis in one-pot methods,and the advantages and limitations of one-pot synthesis are also dis-cussed.
