4-(3-羟基苯基)-2,6-二甲基-1,4-二氢吡啶-3,5-二羧酸乙酯的合成和晶体结构

Synthesis and Crystal Structure of Diethyl 4-(3-hydroxyphenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate

标题化合物C19H23NO5由间羟基苯甲醛、碳酸氢铵、乙酰乙酸乙酯在乙醇溶剂中回流制备。结构通过单晶X-射线衍射法测定,其晶体属三斜晶系,空间群P墿,a=7.4550(15),b=8.9780(18),c=14.099(3),α=80.22(3),β=86.72(3),γ=68.62(3)°,V=865.9(3)3,Z=2,Mr=345.38,Dc=1.325g/cm3,F(000)=368。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R1=0.0633,wR2=0.1709[I>2σ(I)]。在晶体结构中,二氢吡啶环与苯环之间的二面角为90.0(2)°,分子通过氢键形成有隧道的一维超分子结构。

The title compound （C19H23NO5 ） has been synthesized by the reaction of 3-hydroxybenzaldehyde, ethyl acetoacetate and ammonium hydrogen carbonate in the solution of ethanol under reflux. Its structure was determined by single crystal X-ray diffraction. The crystal is triclinic, space group Pī, α = 7.4550（15）, b = 8.9780（18）, c = 14.099（3）A, α = 80.22（3）, β = 86.72（3）, γ = 68.62（3）°, V = 865.9（3）A^3, Z = 2, Mr = 345.38, Dc = 1.325g/cm^3 , F（000） = 368. The structure was solved by direct methods and refined by full-matrix least squares method to the final R1 = 0.0633, ωR2 = 0. 1709 [I 〉 2σ（I）]. X-ray analysis reveals that the dihedral angle between the pyridine and phenyl ring is 90.0 （2）°. The molecule has one-dimensional supramolecular structure with the tunnel through intermoleeular N-H…O and O-H…O hydrogen bonds.