NMR ANALYSIS OF AN OLIGOSACCHARIDE

在瓦里安Inova 600-MHz上进行了~1H-核磁共振分析 分光计。样品用冷冻干燥的方法进行了换氢处理。 从D2O(超声处理半小时，冷冻干燥2X)，以及 然后溶解在0.7mLD2O中进行核磁共振分析(超声处理一半 小时，然后以每分钟3500转的速度离心半小时，然后 将上清液转移到核磁共振管中)。由于这一过程 留下了相当多的不溶性物质，在超声波的过程中 重复D2O、离心和转移，以产生第二个 样品与第一个样品进行比较。1H-核磁共振一维和二维TOCSY(总计 相关光谱学)和NOESY(核Overhauser效应 光谱学)实验，以及1H-13C-gHSQC检测 (梯度异核单量子关联)和-gHMBC (梯度异核多键相关)实验 在第一个样品上以25(C)进行。质子和碳化学 相对于丙酮内标物S测量位移((=2.225 Ppm和29.9ppm)。第二类化合物的1H-核磁共振一维谱 样品的获取纯粹是为了比较光谱特征和 峰值集成。完成了~1H和~(13)C的归属 通过TOCSY和HSQC实验得到，平均重复次数 从HMBC和NOESY的解释中阐明结构 实验。

1H-NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O (2 X by sonication for a half hour, and lyophilization), and then dissolved in 0.7 mL D2O for NMR analysis (sonication for a half hour, followed by centrifugation at 3500 rpm for a half hour and transfer of the supernatant to the NMR tube). Since this procedure left considerable insoluble material, the process of sonication in D2O, centrifugation, and transfer was repeated to produce a second sample for comparison with the first. 1H-NMR 1-D and 2-D TOCSY (total correlation spectroscopy), and NOESY (nuclear Overhauser effect spectroscopy) experiments, as well as 1H-detected 1H-13C-gHSQC (gradient heteronuclear single quantum correlation) and -gHMBC (gradient heteronuclear multiple-bond correlation) experiments were performed at 25(C on the first sample. Proton and carbon chemical shifts were measured relative to internal acetone standard s ((=2.225 ppm and 29.9 ppm, respectively). A 1H-NMR 1-D spectrum of the second sample was obtained purely for comparison of spectral features and peak integration. Complete 1H- and 13C-resonance assignments were obtained by TOCSY and HSQC experiments, and the average repeating structure elucidated from interpretation of the HMBC and NOESY experiments.