微波辐射下2,7,7-三甲基-3-乙氧羰基-4-(3-硝基苯基) -5-氧代-1,4,5,6,7,8-六氢喹啉的合成和晶体结构  

Synthesis andCrystal Structure of 2,7,7-Trimethyl-3-ethoxycarbonyl- 4-(3-nitrophenyl)-5-oxo-1,4,5,6,7,8-hexahydroquinoline under Microwave Irradiation

作　　者：屠树江[1] 于晨侠[1] 刘晓红[1] 姚昌盛[1] 刘芳 高原[2] 

机构地区：[1]徐州师范大学化学系,江苏徐州221009 [2]深圳大学化学系,广东深圳518060

出　　处：《Chinese Journal of Structural Chemistry》2002年第1期99-102,共4页结构化学（英文）

基　　金：江苏省自然科学基金(BK2001142);江苏省教育厅自然科学基金(01KLB150008)资助项目

摘　　要：标题化合物C21H24N2O5是由间硝基苯甲醛、达咪酮、乙酰乙酸乙酯、醋酸铵在微波辐射下干反应而得。结构通过单晶X-射线衍射法确定,其晶体属斜方晶系,空间群 Pbcn, a =17.953(3), b =15.206(4), c =14.299(3), V =3904.(2)3, Mr =384.42, Z =8, Dc =1.308g/cm3 , m(MoKa) =0.094mm-1, F(000)=1632。晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0493, wR=0.1078。X-射线分析结果表明,吡啶环为船式构象,与之稠合的六元环为信封式构象。The title compound (C21H24N2O5) has been synthesized by the reaction of 3-nitrobenzaldehyde, dimedone, ethyl acetoacetate and ammonium acetate under microwave irradiation without solvent and its structure was determined by single-crystal X-ray diffraction. The crystal is orthorhombic, space group Pbcn with a =17.953(3), b =15.206(4), c =14.299(3), V=3904(2)3, Z =8, Mr =384.42, Dc =1.308Mg/m3, ?(MoKα) =0.094cm-1, F(000) =1632. The structure was solved by direct methods and refined by full-matrix least-squares method to the final R=0.0493, wR =0.1078. X-ray analysis reveals that the prydine ring is of boat conformation and the six-membered ring fused with it is of envelope conformation.

关 键 词：微波辐射 合成 喹啉 晶体结构 1 4-二氢吡啶 

分 类 号：O626[理学—有机化学]