摘要
茚基(芴基)锂与2-溴乙胺氢溴酸盐在乙醚中按2:1物质的量比反应,分别得到2-茚基(芴基)乙胺氢溴酸盐(1)和3,1和3再与水杨醛缩合,分别得到水杨醛缩2-茚基(芴基)乙胺席夫碱2和4.通过~1H NMR,IR,MS和元素分析等手段对产物进行了表征,X射线分析确定了2,4的晶体结构.其中化合物2属于单斜晶系,P2_1/c空间群,a=0.9771(2)nm,b=1.9561(4)nm,c=1.1901(3)nm,β=99.955(5)°,M_r=375.53,V=2.2404(8)nm^3,D_c=1.113g/cm^3,Z=4,F(000)=816,μ=0.066mm^(-1),R_1=0.0769,wR_2=0.1625.化合物4属于三斜晶系,P(?)空间群,a=0.9688(3)nm,b=0.9699(3)nm,c=1.3535(5)nm,α=95.280(7)°,β=105.394(11)°,γ=90.987(12)°,M_r=425.59,V=1.2197(8)nm^3,D_c=1.159g/cm^3,Z=2,F(000)=460,μ=0.069mm^(-1),R_1=0.0589,wR_2=0.1312..
Reaction of indenyl lithium or fluorenyl lithium with 2-bromoethylamine hydrobromide gave two new intermediates 1 and 3 respectively, which were then condensed with 3,5-di-tert-butylsalicylaldehyde to afford two new Schiffbases 2 and 4 respectively. These compounds were characterized by elemental analysis, IR spectra and X-ray structural determination. The crystal of the compound 2 belongs to monoclinic, space group P21/c with cell parameter a=0.9771（2） nm, b= 1.9561（4） nm, c= 1.1901（3） nm, β= 99.955（5）°, Mr=375.53, V=2.2404（8） nm3, Dc= 1.113 g/cm3, Z=4, F（000）=816,/z=0.066 mm-1, R1= 0.0769 and wR2=0.1625. The crystal of the compound 4 belongs to triclinic, P1 space group, a=0.9688（3） nm, b=0.9699（3） nm, c= 1.3535（5） nm, a=95.280（7）°, β=105.394（11）°, y=90.987（12）°, Mr=425.59, V= 1.2197（8） nm3, Dc= 1.159 g/cm3, Z=2, F（000） = 460,/1=0.069 mm-1, R1 =0.0589 and wR2 =0.1312.
出处
《有机化学》
SCIE
CAS
CSCD
北大核心
2011年第4期528-532,共5页
Chinese Journal of Organic Chemistry
基金
苏州市职业大学博士启动基金(No.2009BS01)
青年创新基金(No.201052DYY12)
大学生创新基金(No.2010SZDX11)资助项目
关键词
茚
芴
水杨醛
席夫碱
合成
晶体结构
indene
fluorene
salicylaldehyde
Schiff-base
synthesis
crystal structure
