目的：建立了在水相中,通过微波辅助的多组分反应一步合成吡啶酮衍生物的方法;方法：以芳醛、1,3-二羰化合物、麦氏酸和醋酸氨为起始原料,在水相中,通过微波辅助的多组分反应一步合成吡啶酮及其衍生物.结果：反应在3-8 m in内完成,产率优良81-95%,产物结构经红外,核磁和元素分析得以确证.结论：该方法具有反应时间短,产率高,操作简单,环境友好等优点.
The title compounds have been synthesized via a three-component reaction and their structures were characterized by IR, ^1H NMR, ^13C NMR and X-ray single-crystal diffraction. The crystal of compound 4a belongs to monoclinic, space group P121/c1 with a = 8.575（3）, b = 9.590（3）, c = 21.431（6）A, β = 91.172（3）°, V = 1762.1（9）A^3, Mr = 393.36, Z = 4, Dc= 1.483 g/cm^3, μ（MoKα） = 0.113 mm^-1, F（000） = 816, the final R = 0.0366 and wR = 0.0941. The crystal of compound 4b is of triclinic, space group P-1 with a = 8.6420（17）, b = 9.761（2）, c = 11.132（2） A, α = 97.51（3）, β = 97.86（3）, γ = 92.85（3）°, V = 920.1（3） A^3, Mr = 393.36, Z = 2, Dc = 1.420 g/cm^3, μ（MoKα） = 0.108 mm^-1, F（000） = 408, the final R = 0.0612 and wR = 0.1781. In each molecular structure, the naphthalene rings and pyran rings are almost coplanar with the latter in an envelope conformation. The rings formed by the N-H…O intramolecular hydrogen bonds are almost planar in these compounds. Their crystal packing is stabilized by intermolecular hydrogen bonds together with C-H…π and π-π stacking interactions.
The solvents for the separation of diphenyl and 4-phenylacetophenone were screened with computer according to the solid-liquid equilibrium equation based on UNIFAC.With the predicted separation factor values and selection principle for feasible solvents,the candidates of better solvents were determined as n-heptane,n-hexane,cyclohexane and diisopropyl ether.The solubility and separation factor of the two solid solutes in n-heptane,n-hexane,cyclohexane,diisopropyl ether and ethanol were measured by static equilibrium method.The average relative deviation between the calculated separation factor and experimental data is 16.73%,indicating that the solid-liquid equilibrium equation based on UNIFAC is suitable to select the separation solvent for solid solute mixtures with similar molecule stereoscopic structures.
The title compound 5-cyclopropyl-10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11（6H,10H）-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-（cyclopropylamino）-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138（3）, b = 8.952（2）, c = 17.140（3）A, β = 102.253（3）°, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9（8）A^3, Dc = 1.296 g/cm^3, μ（MoKα） = 0.087 mm^-1, F（000） = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.
