微波辐射下4-(4-羟基-3-甲氧基)苯基-3,3,6,6-四甲基-1,8-二氧代1,2,3,4,5,6,7,8,9,10-十氢吖啶的合成和晶体结构

标题化合物C24H29NO4?1/2C2H5OH稨2O)由香兰素、5,5-二甲基-1,3-环己二酮、醋酸铵在微波辐射下干反应并经95%乙醇重结晶而得C24H29NO4穀2(C2H5OH稨2O)晶体。结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/n, a = 9.810(2), b = 14.516(3), c = 17.008(3) ? b = 101.03(2), V = 2377.2(8) ?, Z = 4, Mr = 427.52, Dc = 1.195 g/cm3 , m(MoKa) = 0.082 mm-1, F(000) = 920。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 = 0.0406, wR = 0.0892。X-射线衍射分析结果表明,吡啶环和与之稠合的2个六员环均为信封式构象。

Synthesis and Crystal Structure of 9-(3-Methoxy-4-hydroxyphenyl)-3, 3, 6, 6- tetramethyl-1, 2, 3, 4, 5, 6, 7, 8, 9, 10-decahydroacridine-1, 8-dione

The title compound [C24H29NO4?1/2C2H5OH稨2O)] has been obtained by the reaction of 4-hydroxy- 3-methoxybenzaldehyde, dimidone and ammounium acetoacetate under microwave irradiation without solvent and recrystallized from 95% ethanol. Its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 9.810(2), b = 14.516(3), c = 17.005(3) ? ?= 101.03(2), V = 2377.2(8) 3, Z = 4, Mr = 427.52, Dc = 1.159 g/cm3, ?MoK? = 0.082 mm-1 and F(000) = 920. The structure was solved by direct methods and refined by full-matrix least-squares methods to the final R = 0.0406 and wR = 0.0892. X-ray analysis reveals that the pyridine ring and two six-membered rings connected to it are envelope conformation.