摘要
对长春西汀的半合成工艺进行了研究.长春胺经氢氧化钠水解得到长春胺酸,再以长春胺酸为原料,经浓硫酸脱水、酯化得到长春西汀.研究了两步反应的影响因素,优化了反应条件.结果表明,水解反应较佳的条件为:n长春胺∶n氢氧化钠=1∶1.2,15倍质量的乙醇为溶剂,60℃水解2 h;脱水酯化反应较佳的条件为∶m长春胺酸∶m浓硫酸∶m乙醇=1∶2∶20,78℃反应8 h.在该条件下,长春西汀半合成收率达90.7%,色谱纯度达98.5%.通过元素分析、核磁、红外对产物结构进行了表征.
The semi-synthetic process of Vinpocetine has been investigated in this study. The raw material Vincamine acid was produced from Vincamine by sodium hydroxide hydrolysis. Vinpocetine was obtained from Vincamine acid by dehydration and esterification under sulfuric acid. The influence factors of two steps were investigated. The yield and purity of Vinpocetine were 90. 7% and 98.5%, respectively, under the optimal hydrolysis conditions ： n（Vincamine） ： n（NaOH） = 1 ： 1.2, 15-time mass of ethanol as solvent; hydrolysis temperature 60℃ ; hydrolysis time 2 h, and dehydrate-esterification conditions： m （Vincamine acid） ： m（ H2SO4 ） ： m（ethanol） = 1： 2： 20, reaction temperature 78℃, reaction time 8 h. The structure of the product was identified by elemental analysis, 1H-NMR, IR.
出处
《暨南大学学报（自然科学与医学版）》
CAS
CSCD
北大核心
2012年第1期65-68,共4页
Journal of Jinan University(Natural Science & Medicine Edition)
关键词
长春胺
长春西汀
合成
工艺
Vincamine
Vinpocetine
synthesis
technology
