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

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。

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

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.