叶酸有关物质H的合成制备  

Synthesis and Preparation of the Related Substances H of Folic Acid

作　　者：刘露 张仲景 陈天松 庞正查 Liu Lu;Zhang Zhongjing;Chen Tiansong;Pang Zhengcha(Zhejiang Shengda Bio-pharm Co.,Ltd.,Taizhou 317200,China)

机构地区：[1]浙江圣达生物药业股份有限公司

出　　处：《广东化工》2019年第23期34-34,22,共2页Guangdong Chemical Industry

摘　　要：为控制叶酸的质量,本研究合成制备了叶酸欧洲药典(EP9.5)的有关物质H,(2S)-2-[4-[(4S)-4-[4-[[(2-氨基-4-氧代-1,4-二氢喋啶-6-基)-甲基]氨基]苯甲酰氨基]-4-羧基丁酰胺基]苯甲酰氨基]戊二酸。以叶酸,对氨基苯甲酰谷氨酸为原料,经缩合反应,得到杂质H粗品,再经制备色谱法分离,得到了纯度98%以上的杂质H,并由HRMS、1H NMR、13C NMR和DEPT-135进行结构确证,可作为叶酸质量控制的杂质对照品。In order to control the quality of folic acid, this study synthesized and prepared the folic acid European Pharmacopoeia(EP9.5) related substances H,(2 S)-2-[4-[(4 S)-4-[4-[[(2-Amino-4-oxo-1,4-dihydropteridin-6-yl)-methyl]amino]benzoylamino]-4-carboxybutyramido]benzoylamino]-glutaric acid. Using folic acid and p-amino-benzoylglutamic acid as raw materials, the crude product of impurity H was obtained by condensation reaction, and then separated by preparative chromatography to obtain impurity H with a purity of 98 % or more. The structures of impurity H were confirmed by HRMS, 1 H NMR, 13 C NMR and DEPT-135. And can be used as impurity for control of quality.

关 键 词：叶酸 有关物质 合成 制备色谱 

分 类 号：TQ[化学工程]