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在(S)-氨基丙醇及(R)-氨基丙醇手性臂的作用下,(M/P)-4,4’-二甲氧基-5,6,5’,6’-二次甲二氧基-2-甲酸酯-2’-甲酰氨联苯经构型转化,制备了光学纯轴手性联苯化合物(P,S)-3a和(M,R)-3b.测定了(P,S)-3a的晶体结构及CD光谱.结果表明,化合物(P,S)-3a晶体属单斜晶系,P2(1)空间群,晶胞参数为a=12.122(2),b=8.9911(18),c=12.779(3),β=112.38(3)°,在晶体中存在两组分子间氢键相互作用,一组氢键由羟基氢与另一分子酰胺基团的羰基氧组成O—H…O,另一组由酰胺基团的NH与另一分子酰胺基团的羰基氧构成N—H…O,每一分子通过四个氢键与另外两个分子相连,构成棒状结构.由CD光谱确定了(M,R)-3b的立体构型.此外,由(P,S)-3a合成了轴手性化合物(P)-2,2’-二羟甲基-4,4’-二甲氧基-5,6,5’,6’-二亚甲二氧基-联苯(6a).
Under the action of (S) -aminopropanol and (R) -aminopropanol chiral arms, (M / P) -4,4’-dimethoxy-5,6,5 ’, 6’- (P, S) -3a and (M, R) -3b (P, S) -3b were prepared via conformational conversion of methyldicarboxylate- . The crystal structure and CD spectra of (P, S) -3a were determined. The results show that the crystal of (P, S) -3a belongs to the monoclinic space group P2 (1) with unit cell parameters of a = 12.122 2), b = 8.9911 (18), c = 12.779 (3), β = 112.38 (3) °. There are two groups of intermolecular hydrogen bonding interactions in the crystal. One group of hydrogen bonds is formed by the interaction of hydroxyl hydrogen with another molecule of amide The carbonyl oxygen of the group constitutes O-H ... O, and the other group consists of N-H ... O of the NH group of the amide group and the carbonyl oxygen of the other amide group, and each molecule passes through four hydrogen bonds with the other two (C, R) -3b was determined by CD spectra.Furthermore, (P, S) -3a was synthesized by the axial chiral compound (P) -2,2’-bis Hydroxymethyl-4,4’-dimethoxy-5,6,5 ’, 6’-dimethylenedioxy-biphenyl (6a).