有效的[4+1]/[3+2+1]双环化反应构建茚并氧杂蒽杂环骨架及其晶体结构  

Effective Indeno Xanthene Heterocycle Compound and Crystal Structure Based on [4 + 1]/[3 + 2 + 1]Dicyclic Reaction

作　　者：高侠[1] 朱晓彤[2,3] 

机构地区：[1]江苏省徐州医药高等职业学校,江苏徐州221116 [2]徐州医科大学公共教育学院,江苏徐州221004 [3]中国矿业大学化学化工学院,江苏徐州221116

出　　处：《化学试剂》2017年第8期874-878,共5页Chemical Reagents

基　　金：徐州市科技发展计划资助项目(XM13B067)

摘　　要：茚并氧杂蒽类化合物C24H28O5是由邻苯二甲醛和5,5-二甲基-1,3-环己二酮在醋酸溶剂中,于室温下搅拌一步法反应制得,通过单晶X-射线衍射法测定其结构。该晶体属单斜晶系,空间群P2(1),晶胞参数a=1.006 92(11)nm,b=1.021 73(12)nm,c=2.430 6(2)nm,V=2.500 6(5)nm^3,Z=4,晶胞密度Dc=1.247 mg/m^3,吸收系数μ=0.087 mm^(-1),单胞中电子的数目F(000)=1 008,分子量Mr=469.56(单晶中包含一分子溶剂DMF)。晶体结构经全矩阵最小二乘法对各原子参数进行修正,最终得到的偏离因子为R=0.061 9,ωR=0.090 4。在晶体结构中新形成的茚环呈现信封式构象,同时形成的吡喃环显示为扭船式构象。The indeno xanthene heterocyele compound C24H28O5 has been one-step synthesized by the reaction of o-phthalaldehyde and 5,5-dimethyl-1,3-cyclohexanedionein acetic acid by stirring at room temperature.The structure was determined by single crys- tal X-ray diffraction.The crystal is monoclinic, space group P2（ 1 ） ,with Mr = 469.56（ a molecular solvent of DMF was included in the crystal） ,a= 1. 006 92（ 11） nm,b=1.021 73（12） nm,c=2.4306（2） nm,V=2.5006（5） nm3,Z=4,D,=1.247 mg/m3, μ=0. 087 mm-1 ,F（000）= 1 008.The stnacture was solved by direct methods and refined by full-matrix least squares method to the final R=0. 061 9,ωR= 0.094. X-Ray analysis reveals that the newly formed pyran-ring in the crystal structure is the skew boat conformation,while the indene ring is the envelope conformation.

关 键 词：简便合成 室温 一步法 晶体结构 

分 类 号：O626[理学—有机化学]