摘要
以硝基甲烷-13 C为原料合成D-半乳糖-1-13 C。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%,13 C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(1 H NMR)对所得产物进行结构表征,确定产物结构为D-半乳糖-1-13 C。
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.
出处
《同位素》
CAS
2012年第4期219-227,共9页
Journal of Isotopes
基金
国家高技术研究发展计划项目(2008AA02Z427)