| 1254513-75-1

• 分子结构分类: 有机化合物 - 有机杂环化合物 - 哌啶类
• CAS: 1254513-75-1
• 化学式: C₃₃H₆₉N₄O₇
• 分子量: 633.933
• InChiKey: HETOEWNKFYKNKT-UHFFFAOYSA-N

计算性质

• 辛醇/水分配系数(LogP)：
  1.6
• 重原子数：
  44
• 可旋转键数：
  11
• 环数：
  3.0
• sp3杂化的碳原子比例：
  1.0
• 拓扑面积：
  113
• 氢给体数：
  2
• 氢受体数：
  9

反应信息

• 作为反应物：
  描述：

  在 四丁基硫酸氢铵 、 sodium hydroxide 、 erbium(III) triflate 作用下， 以 水 、 乙腈 为溶剂， 反应 168.0h， 生成
  参考文献：
  名称：

  Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR

  摘要：

  We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25-30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2-6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92-128 for cross-polarized C-13 NMR signals from N-15,C-13-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6-3.8 s for H-1 spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute C-13 NMR signal amplitudes and build-up times, are approximately 2-4 times lower than with the best triradicals. Published by Elsevier Inc.

  DOI：

  10.1016/j.jmr.2014.05.002
• 作为产物：
  描述：

  阻聚剂701 在 lithium perchlorate 、 四丁基硫酸氢铵 、 sodium hydroxide 作用下， 以 水 、 乙腈 为溶剂， 生成
  参考文献：
  名称：

  Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR

  摘要：

  We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25-30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2-6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92-128 for cross-polarized C-13 NMR signals from N-15,C-13-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6-3.8 s for H-1 spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute C-13 NMR signal amplitudes and build-up times, are approximately 2-4 times lower than with the best triradicals. Published by Elsevier Inc.

  DOI：

  10.1016/j.jmr.2014.05.002

文献信息

• Succinyl-DOTOPA: An effective triradical dopant for low-temperature dynamic nuclear polarization with high solubility in aqueous solvent mixtures at neutral pH
  作者：Wai-Ming Yau、Jaekyun Jeon、Robert Tycko

  DOI：10.1016/j.jmr.2019.106672

  日期：2020.2

  dopant for dynamic nuclear polarization (DNP) experiments in frozen solutions at low temperatures. Compared with previously described DOTOPA derivatives, succinyl-DOTOPA has substantially greater solubility in glycerol/water mixtures with pH > 4 and therefore has wider applicability. Solid state nuclear magnetic resonance (ssNMR) measurements at 9.39 T and 25 K, with magic-angle spinning at 7.00 kHz, show

  我们报告了基于氮氧化合物的三基化合物琥珀酰-DOTOPA 的合成及其作为低温冷冻溶液中动态核极化 (DNP) 实验掺杂剂的性能表征。与之前描述的 DOTOPA 衍生物相比，琥珀酰-DOTOPA 在 pH > 4 的甘油/水混合物中具有更大的溶解度，因此具有更广泛的适用性。固态核磁共振 (ssNMR) 在 9.39 T 和 25 K 下测量，魔角以 7.00 kHz 旋转，表明 DNP 增强的交叉极化 13C ssNMR 信号的建立时间更短，信号幅度更大对于含有琥珀酰-DOTOPA 的 L-脯氨酸的甘油/水溶液比含有双自由基 AMUPol 的溶液具有 15 mM 或 30 mM 的电子自旋浓度，导致 DNP 带来更大的净灵敏度增益。在 90 K 的类似测量中，AMUPol 产生更高的净灵敏度，这显然是由于其更长的电子自旋晶格和自旋自旋弛豫时间。一维和二维 13C ssNMR 在 25 K 下对