摘要
以盐酸吡哆醇(VB6)为起始原料,经氧化反应、醛基保护、磷酸酯化和水解反应合成了磷酸吡哆醛。对MnO2氧化VB6、吡哆醛席夫碱磷酸酯化,以及水解后磷酸吡哆醛结晶等条件进行了研究。结果表明:MnO2氧化VB6的最优条件反应是在质量分数6%盐酸溶液中进行,VB6和MnO2的摩尔比为1∶2,反应温度15℃,反应时间6 h。吡哆醛席夫碱的最优磷酸酯化试剂为加入了少量水(质量分数3%)的多聚磷酸。磷酸吡哆醛席夫碱的水解溶液经强酸性阳离子交换树脂酸化后,冷冻干燥得到磷酸吡哆醛,解决了磷酸吡哆醛结晶难的问题。整个工艺路线易于工业化生产,磷酸吡哆醛的总收率达到61.6%。
Pyridoxal phosphate was synthesized from pyridoxine hydrochloride(VB6)by oxidation,aldehyde protection,phosphate esterification and hydrolysis. The conditions of oxidizing VB6 by MnO2,phosphate esterification of the pyridoxine Schiff base and crystallization of pyridoxal phosphate from water were investigated. The result shows that optimal oxidation of VB6 is carried out in hydrochloric acid solution of 6%,the mole ratio of VB6 and MnO2 of 1∶2,at the reaction temperature of 15 ℃ and the reaction time of 6 h.Polyphosphoric acid with 3%(mass fraction of water)is the optimal phosphate esterification reagent for the pyridoxine Schiff base. The hydrolysis solution of pyridoxal phosphate Schiff base is acidified with strong acid cation exchange resin,followed by freeze-drying to obtain pyridoxal phosphate,which solves the problem of difficult crystallization of pyridoxal phosphate. The entire process is easy to industrialize,and the total yield of pyridoxal phosphate reaches 61.6%.
作者
宣良明
胡旭
冯权武
卢伟
尹传奇
XUAN Liangming;HU Xu;FENG Quanwu;LU Wei;YIN Chuanqi(School of Chemistry and Environmental Engineering,Wuhan Institute of Technology,Wuhan 430205,China;Hubei Huisheng Pharmaceutical Co.,Ltd,Xianning 437000,China)
出处
《武汉工程大学学报》
CAS
2020年第4期355-359,共5页
Journal of Wuhan Institute of Technology
基金
湖北省教育厅项目(B2017053)
武汉工程大学研究生教育创新基金(CX2018142)。
关键词
盐酸吡哆醇
氧化反应
强酸性阳离子交换树脂
冷冻干燥
磷酸吡哆醛
合成工艺
pyridoxine hydrochloride
oxidation reaction
strong acid cation exchange resin
freeze drying
pyridoxal phosphate
synthesis process
