^(13)C呼吸试剂D-木糖-U-^(13)C_5的合成

Synthesis of D-Xylose-U-^(13)C_5

以D-葡萄糖-U-13 C6为起始原料,采用减碳法经双丙酮保护、选择性酸水解、氧化、还原和碱水解五步合成D-木糖-U-13 C5,总产率为38.6%(以D-葡萄糖-U-13 C6计)。对每步产物使用相应的气相色谱(GC)、气质联用仪(GC-MS)、液相色谱(HPLC)和液质联用仪(LC-MS)进行表征。分析结果表明,每步反应中的产物均为目的产物,同位素丰度和纯度都符合要求,最后一步的产物为D-木糖-U-13 C5,其13 C丰度为99.1%,化学纯度为99.9%,符合13 C呼吸试验的要求。

D-Xylose-U-13C5 was synthesized with D-glucose-U-13C6 as starting material via process of protection with double acetone,selective hydrolysis with acid,oxidation,reduction and hydrolysis with base.The total yield of D-Xylose-U-13C5 was 38.6% base on D-glucose-U-13C6.The target compound and their intermediates were analyzed and characterized by GC,GC-MS,HPLC and LC-MS,accordingly.The results showed that their isotopic abundance and purity could meet the required specification.The structure of final product was D-Xylose-U-13C5,13C abundance was 99.1%,and chemical purity was 99.9%,which were high enough for use in 13C breath test.