以4-溴苯腈为起始原料经过Suzuki偶联反应、Miyanra硼化反应等合成了3’-(4-溴萘-1-基)[1,1’-联苯基]-4-腈(Ⅲ),利用~1 H NMR、^(13) C NMR对其结构进行了表征.考察了反应温度、膦配体及碱等因素对3-溴-4’-腈基联苯(Ⅰ)收率的影响.结...以4-溴苯腈为起始原料经过Suzuki偶联反应、Miyanra硼化反应等合成了3’-(4-溴萘-1-基)[1,1’-联苯基]-4-腈(Ⅲ),利用~1 H NMR、^(13) C NMR对其结构进行了表征.考察了反应温度、膦配体及碱等因素对3-溴-4’-腈基联苯(Ⅰ)收率的影响.结果表明,55℃为最佳反应温度、Pd_2(dba)_3作为催化剂、三(对甲苯基)膦为配体,化合物Ⅰ收率最高,达到92.3%.通过TG、荧光发射光谱研究了化合物Ⅲ的发光效率和稳定性.化合物Ⅲ具有很好的热稳定性,失重5%的温度为321.5℃.展开更多
The crystal structure of 5-{[(4′-heptoxy-biphenylyl-4-yl)oxy]carbonyl}-1-pentyne({A3E′O7}) was investigated by wide angle X-ray diffraction(WAXD), transmission electron microscope(TEM) and atom force microscope(AFM)...The crystal structure of 5-{[(4′-heptoxy-biphenylyl-4-yl)oxy]carbonyl}-1-pentyne({A3E′O7}) was investigated by wide angle X-ray diffraction(WAXD), transmission electron microscope(TEM) and atom force microscope(AFM). The structures of A3E′O7 solution-crystal and melt-crystal are the same. The crystals belong to the monoclinic P112/m space group, the cell parameters are {a0.589 nm}, b0^771 nm, c4.75 nm, αβ90° and γ93.8°, the calculated cell density is {1.167 g/cm+3}.展开更多
文摘以4-溴苯腈为起始原料经过Suzuki偶联反应、Miyanra硼化反应等合成了3’-(4-溴萘-1-基)[1,1’-联苯基]-4-腈(Ⅲ),利用~1 H NMR、^(13) C NMR对其结构进行了表征.考察了反应温度、膦配体及碱等因素对3-溴-4’-腈基联苯(Ⅰ)收率的影响.结果表明,55℃为最佳反应温度、Pd_2(dba)_3作为催化剂、三(对甲苯基)膦为配体,化合物Ⅰ收率最高,达到92.3%.通过TG、荧光发射光谱研究了化合物Ⅲ的发光效率和稳定性.化合物Ⅲ具有很好的热稳定性,失重5%的温度为321.5℃.
文摘The crystal structure of 5-{[(4′-heptoxy-biphenylyl-4-yl)oxy]carbonyl}-1-pentyne({A3E′O7}) was investigated by wide angle X-ray diffraction(WAXD), transmission electron microscope(TEM) and atom force microscope(AFM). The structures of A3E′O7 solution-crystal and melt-crystal are the same. The crystals belong to the monoclinic P112/m space group, the cell parameters are {a0.589 nm}, b0^771 nm, c4.75 nm, αβ90° and γ93.8°, the calculated cell density is {1.167 g/cm+3}.
