共查询到20条相似文献,搜索用时 125 毫秒
1.
2.
3.
4.
5.
6.
7.
8.
以离子液体[Hnmp]HSO4为催化剂, 在无溶剂条件下催化芳香醛、2-氨基苯并噻唑和2-萘酚合成一系列的2 -氨基苯并噻唑-芳甲基-2-萘酚. 该方法条件温和, 反应时间短, 产率高和对环境友好. 此外催化剂可以方便地回收, 且循环使用四次其催化活性并没有显著降低. 目标产物经过了1H NMR, IR, MS和元素分析确证. 相似文献
9.
合成一类新型非茂钛 乙酰基萘酚钛配合物 [O ,O]nTiCl4 n,该系列催化剂可在较温和的条件下催化乙烯聚合 ,其催化活性在 10 4gPE (molTi·h)左右 ;由于配合物在溶剂中存在缔合现象 ,是导致活性降低和产物分子量分布加宽 .通过将乙酰基萘酚钛配合物 [O ,O]nTiCl4 n负载到MgCl2 上 ,可以大大提高催化活性 ,使之达到 10 6 gPE (molTi·h)以上 .负载后的催化剂反应平稳 ,寿命较长 .而且反应的铝钛比较低 ,并可以使用烷基铝作助催化剂 .负载催化剂所得的聚合物分子量要高于均相所得聚合物分子量 ,且分子量分布变窄 .用粉末X 衍射考察了负载催化剂的结构 .通过X 射线光电子能谱的分析 ,考察负载前后钛、镁、氯元素的电子结合能变化对催化乙烯聚合活性的影响 . 相似文献
10.
11.
A solvent compensation method based on flow injection analysis is used to obtain high quality nuclear magnetic resonance (NMR) spectra during solvent gradients. Using a binary solvent system containing D2O and CD3OD, NMR line broadening and chemical shift changes are observed with a 10% methanol per min solvent composition gradient. However, by creating a second equal but reverse gradient and combining the two solvent gradients before the NMR detector, the composition of solvent reaching the NMR flow cell is kept constant. We demonstrate a system using flow injection analysis of combining solvent gradients and show constant NMR spectral performance as a function of time as the combined flow has a constant solvent composition irrespective of the initial solvent gradient. Using this approach, methods can be developed to measure high quality NMR spectra during on-flow gradient LC-NMR experiments. The ultimate ability of this approach depends on the ability to compensate for the disturbance of the solvent gradient and reverse gradient by a pair of LC columns (the analytical and reverse gradient columns). 相似文献
12.
NMR J-couplings across hydrogen bonds reflect the static and dynamic character of hydrogen bonding. They are affected by thermal and solvent effects and can therefore be used to probe such effects. We have applied density functional theory (DFT) to compute the NMR (n)J(N,H) scalar couplings of a prototypical Chagas disease drug (metronidazole). The calculations were done for the molecule in vacuo, in microsolvated cluster models with one or few water molecules, in snapshots obtained from molecular dynamics simulations with explicit water solvent, and in a polarizable dielectric continuum. Hyperconjugative and electrostatic effects on spin-spin coupling constants were assessed through DFT calculations using natural bond orbital (NBO) analysis and atoms in molecules (AIM) theory. In the calculations with explicit solvent molecules, special attention was given to the nature of the hydrogen bonds formed with the solvent molecules. The results highlight the importance of properly incorporating thermal and solvent effects into NMR calculations in the condensed phase. 相似文献
13.
14.
结合样品核磁测试结果,以具体实例的形式,总结了核磁样品分析的基本要求,分析了核磁管和氘代试剂的选择、样品制备及pH值等因素对核磁测试结果的影响,并提出了样品最优测试条件:核磁管管体内外表面要足够光洁均匀,在高温条件下,优先选用升温核磁管.尽量选择小支封装氘代试剂,降低水峰的影响,并且应考虑样品的性质,避免试剂与测试样品发生反应.样品必须与溶剂充分混合均匀,样品量要在溶液粘度与灵敏度之间做好平衡.在分析与氧、氮和硫共价相连的氢原子时,应该选择恰当的pH溶液.以上研究结果可以为其它样品核磁测试提供借鉴指导. 相似文献
15.
16.
采用核磁共振波谱(NMR)研究了二苯基甲烷二异氰酸酯(MDI)在稀溶液中的水解反应机理.将同一MDI样品分别溶解在氘代氯仿、氘代丙酮和加入少量水分的氘代二甲基亚砜溶剂(DMSO)中,进行核磁共振氢谱(1H NMR)、核磁共振碳谱(13C NMR)测试.结果显示,MDI在含水的DMSO溶剂中测得的谱图与氘代氯仿、氘代丙酮中的差别显著.对该溶液进行了13C-1H异核近程相关(HMQC)、13C-1H异核远程相关(HMBC)及碳原子级数(DEPT 135)测试,并利用经验公式对其进行了详细归属,确认了反应产物的结构.分析得知MDI在含水溶剂中迅速反应,异氰酸酯基转化为脲基和氨基基团.异氰酸酯与水反应生成氨基基团,其与异氰酸酯反应活性比水高,对位取代氨基与水的竞聚率比值为7.1,邻位为1.4,对位取代氨基活性约是邻位的5倍. 相似文献
17.
Summary: Temperature-induced and solvent composition-induced phase separation in solutions of poly(N-isopropylmethacrylamide) (PIPMAm) and other thermoresponsive polymers as studied by NMR and infrared (IR) spectroscopy is discussed. The fraction p of phase-separated units (units with significantly reduced mobility) and subsequently, e.g., thermodynamic parameters characterizing the coil-globule phase transition induced by temperature, were determined from reduced integrated intensities in high-resolution 1H NMR spectra. This approach can be especially useful in investigations of phase separation in solutions of binary polymer systems. Information on behaviour of water during temperature-induced phase transition was obtained from measurements of 1H NMR relaxation times of HDO molecules. NMR and IR spectroscopy were used to investigate PIPMAm solutions in water/ethanol (D2O/EtOH) mixtures where the phase separation can be induced by solvent composition (cononsolvency). Some differences in globular-like structures induced by temperature and solvent composition were revealed by these methods. 相似文献
18.
以THF为溶剂, CuI/TMEDA为催化剂,四乙酰溴代葡萄糖与芳基溴化镁经取代反应合成了芳基葡萄糖碳苷(2a~2c),其结构经1H NMR和13C NMR确证。该方法立体选择性较好。在最佳反应条件(THF为溶剂,10% CuI和10% TMEDA为催化剂,于0 ℃反应至终点)下,2a~2c的收率为58%~71%, α/β为1/6.5~1/7.1。 相似文献
19.
This paper describes the first coupling of a commercial capillary HPLC system with a diode array spectrophotometric detector and a custom-built nuclear magnetic resonance (NMR) flow microprobe. The eluent from a 3-microm diameter C18 HPLC column is linked to a 500 MHz 1H-NMR microcoil probe with an observe volume of 1.1 microl. The separation and structurally-rich detection of a mixture of terpenoids under both isocratic and gradient solvent elution conditions is presented. The lowest limits of detection yet reported for capillary HPLC on-line measurement (i.e., 37 ng for alpha-pinene) are achieved with this system. The complementary nature of diode array and NMR detection allows stopped-flow data collection from analytes which would otherwise go unnoticed in continuous-flow NMR. Moreover, stopped-flow NMR data is presented for the detection of a trace (sub-nmol) impurity in the sample mixture. Since NMR signals degrade and shift during solvent gradients, flow injection analysis studies are conducted with injected solvent plugs differing in mobile phase composition. The NMR signal degradation accompanying these injections is largely due to the variance in chemical shift with the solvent composition rather than to changes in magnetic susceptibility of the solvent. Characterization of such effects enables the development of improved NMR probes for the coupling of capillary HPLC and NMR. 相似文献