2,2’-(3-硝基-4-氯苯基)次甲基雙(3-羥基-5,5-二甲基-2-環己烯-1-酮)合成與晶體結構

以3-硝基-4-氯苯甲醛和5,5-二甲基-1,3-環己二酮為原料,二甲基甲酰胺為溶劑,不需催化劑合成一種新的氧雜蒽二酮開環衍生物2,2’-(3-硝基-4-氯苯基)次甲基雙(3-羥基-5,5-二甲基-2-環己烯-1-酮)晶體,確定最佳反應條件是:芳醛和脂肪環酮的摩爾投料比為1∶2,反應溫度為80℃,反應時間為1 h;并對其進行熔點、元素分析、紅外光譜、氫核磁共振及X-射線單晶衍射測定。該晶體為單斜晶系,空間群=P21/n,a=1.95777 (13) nm,b=1.22720 (9) nm,c=1.99687 (14) nm,β=107.719 (2) °,V=4.5700 (6) nm3,Z=8,dC=1.302 g/m3,μ=0.205 mm-1,F (000) =1888。 At the molar ratio of 1:1.2 and 80°C, a novel crystal 2, 2'-(3-nitro-4-chlorobenzyl) methylene bis(3-hydroxy-5, 5-dimethyl-2-cyclohexene-1-one), was synthesized through reacting 3-nitro-4-chlorobenzaldehyde with 5, 5-Dimethyl-1, 3-cyclohexanedione using DMF as the solvent for 1 h in the absence of any catalyst. The structure was characterized by melting points, elemental analysis, IR, 1H NMR and X-ray single crystal diffractometer. The result shows the crystal in monoclinic crystal system and P21/n space group. Crystallographic date: a=1.95777(13) nm, b=1.22720(9) nm, c=1.99687(14) nm, β=107.719(2)°, V=4.5700(6) nm3, Z=8, dC=1.302 g/m3, μ=0.205 mm-1, F(000)=1888