微波辐射下4-(2-氯苯基)-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的合成和晶体结构

标题化合物C14H15ClN2O3是由2-氯苯甲醛、乙酰乙酸乙酯、尿素在TsOH作用下用微波辐射反应得到, 结构通过单晶X-射线衍射法确定, 其晶体属三斜晶系, 空间群P, Mr = 294.73, a = 7.688(1), b = 9.106 (2), c = 11.412(2) ? = 102.963(3), = 105.957(2), g = 102.484(2), V = 714.9(2) ?, Z = 2, Dc = 1.369 g/cm3, = 0.276 mm-1, F(000) = 308, 最终的偏离因子为R = 0.0845, wR = 0.2092。在分子结构中嘧啶环为船式结构, 平面1(苯环)与平面2 ((C(8)C(9) C(10)N(2))之间的两面角为 91.57啊?

Synthesis and Crystal Structure of 4-(2-Chlorophenyl)- 6-methyl-5-ethoxycaronyl-3,4-dihydropyrimidin-2(H)-one under Microwave Irradiation

The title compound (C14H15ClN2O3) was synthesized by the reaction of 2-chlorobenzaldehyde, ethyl acetoacetate, urea and TsOH under microwave irradiation and its structure has been determined by single- crystal X-ray diffraction. The crystal is of triclinic, space group P?with a = 7.688(1), b = 9.106(2), c = 11.412(2) ? =102.963(3), = 105.957(2), = 102.484(2), V = 714.9(2) ?, Z = 2, Mr = 294.73, Dc = 1.369 g/cm3, ?= 0.276 mm-1 and F(000)= 308. The structure was solved by direct methods and refined by full-matrix least-squares technique to the final R = 0.0845 and wR = 0.2092. X-ray analysis reveals that the dihedral angle between planes 1 (benzene ring) and 2(C(8)C(9)C(10)N(2)) is 91.5? The pyrimidine ring is in a boat configuration in the structure.