Department of Chemistry, Brown University, Providence, Rhode Island 02912, United States.
J Org Chem. 2013 Jul 19;78(14):7288-92. doi: 10.1021/jo400839q. Epub 2013 Jul 5.
The solid state structure of lithiated (S)-N(1),N(1)-bis(2-methoxyethyl)-N(2),3-dimethylbutane-1,2-diamine, which is a chiral amide base synthesized from (S)-valine was determined by single-crystal X-ray diffraction. The complex in solution state is also characterized by a variety of NMR experiments including diffusion-ordered NMR spectroscopy (DOSY) with diffusion coefficient-formula weight correlation analyses and other one- and two-dimensional NMR techniques by dissolving the crystal in toluene-d8. The crystallography and NMR results suggest that the chiral amide is dimeric in both solid and solution states.
（S）-N（1），N（1）-双（2-甲氧基乙基）-N（2），3-二甲基丁烷-1,2-二胺的锂化固体状态结构通过单晶 X 射线衍射确定，该化合物是由（S）-缬氨酸合成的手性酰胺碱。通过在甲苯-d8 中溶解晶体，还通过各种 NMR 实验（包括具有扩散系数-分子量相关分析的扩散排序 NMR 光谱学（DOSY））和其他一维和二维 NMR 技术对溶液状态下的配合物进行了表征。晶体学和 NMR 结果表明，手性酰胺在固态和溶液态下均为二聚体。
