D-半乳糖-1-13C的合成与表征

Synthesis and Characterization of D-Galactose-1-13C

  • 摘要: 以硝基甲烷13C为原料合成D-半乳糖-1-13C。采用分离中间体硝基糖醇的方式,简便拆分差向异构体D-半乳糖和D-塔罗糖,合成产物的总产率为42.6%,13C丰度为99.1%,光学纯度为100%,化学纯度为99.7%。以高效液相色谱蒸发散射光检测器(HPLC-ELSD)、液相色谱-质谱联用仪(LC-MS)和核磁共振(1H NMR)对所得产物进行结构表征,确定产物结构为D-半乳糖-1-13C。

     

    Abstract: D-Galactose-1-13C was synthesized with nitromethane 13C as starting material. The separation was performed of the epimers of nitro D-Galactitol and nitro D-talitol, which resulted in D-Galactose being obtained and the resolution of the epimers of D-Galactose and D-taltose being avoidance. D-Galactose-1-13C was characterized by HPLC-ELSD, LC-MS and 1H NMR. The fine structure and 13C abundance of it were done by LC-MS and 1H NMR. The yield of 13C-labeled D-Galactose was 42.6% with 99.1% 13C abundance, 100.0% optical purity and 99.7% chemical purity.

     

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