一种甲苯磺酸盐核磁共振谱峰归属与晶体制备  

Assigning Peaks in NMR Spectra and Preparation Crystals of a Sort of Tosylates

作　　者：庞子博[1] 孟大磊[1] 武聪[1] 徐永宽[1] 程红娟[1] 洪颖[1] 杨丹丹[1] 

机构地区：[1]中国电子科技集团公司第四十六研究所,天津300220

出　　处：《硅酸盐学报》2016年第4期545-549,共5页Journal of The Chinese Ceramic Society

摘　　要：通过两步有机反应制备出4-N,N-二甲胺基-4’-N’-甲基-氮杂茋的对甲苯磺酸盐（DAST）粉体,并利用重结晶法进行提纯。通过DAST的二维核磁共振（2D NMR）中同核相关谱（correlated spectroscopy,COSY）、异核单量子相干谱（heteronuclear single-quantum coherence,HSQC）和异核多键相关谱（heteronuclear multiple-bond correlation,HMBC）进行表征,实现了^1H和^13C NMR谱峰的完全归属,确证了DAST分子结构。使用经提纯后的DAST粉体配制其甲醇溶液,通过溶液降温法自发成核过程生长出尺寸为（1～3）mm×（1～3）mm×（0.3～0.6）mm的DAST晶体。4-N,N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） powder was firstly synthesized via two-step organic reaction and then purified via recrystallization. The DAST powder was characterized by 2D nuclear magnetic resonance （2D NMR） with the correlated spectroscopy （COSY）, heteronuclear single-quanaun coherence （HSQC） and heteronuclear multiple-bond correlation （HMBC）. The full assignments of peaks in the ^1H and ^13C NMR spectra were achieved and the molecular structure of DAST was verified. The purified DAST powder was used to prepare its solution in methanol, and DAST crystals with the size of （1-3） mm× （1-3）mm× （0.3-0.6）mm were grown in a spontaneous nucleation process by a solution temperature-reduction method.

关 键 词：对甲苯磺酸盐 有机非线性光学晶体 核磁共振 谱峰归属 晶体生长 

分 类 号：O782.1[理学—晶体学]