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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。
The 4-N, N-dimethylamino-4’-N’-methyl-azepine p-toluenesulfonate (DAST) powder was prepared by two steps of organic reaction and purified by recrystallization. Nuclear magnetic resonance (Doppler correlation spectroscopy, COZY, heteronuclear single-quantum coherence (HSQC) and heteronuclear multiple-bond correlation, HMBC), the complete assignment of the 1H and 13C NMR peaks was confirmed, confirming the DAST molecular structure. The purified DAST powder was used to prepare the methanol solution, and the DAST crystals with sizes of (1 ~ 3) mm × (1 ~ 3) mm × (0.3 ~ 0.6) mm were spontaneously nucleated by the solution cooling method.