摘要
目的开发稳定同位素氘代标记吡罗昔康-d_3的合成方法。方法以邻苯甲酰磺酰亚胺为原料,氘代碘甲烷为氘代标记试剂,经过烷基化、重排、氘代甲基化与酯的氨解得到氘代标记的吡罗昔康-d_3。结果总收率为26.6%,化学纯度为99.2%,氘代丰度为99.3%,目标化合物结构经质谱、核磁共振等表征确定。结论该4步合成路线方法简单,原料易得、反应条件易于控制,产品可用于其在药代动力学方面的研究。
Objective To develop a method of the synthesis of the deuterium-labeled piroxicam-d3.Methods Piroxicam-d3 was synthesized from saccharin via alkylation,rearrangement,deuterated methylation and ammoniation.Deuterated methyl iodide was used as the labeling reagent.Results The total yield was 26.6%,and the structure of the target compound was confirmed by MS and NMR.Its chemical purity was 99.2%and the deuterated abundance was 99.3%.Conclusion The four-step syntheses can be simple and efficient,and all starting materials used in this study can be commercially available.It can be used as an internal standard for pharmacological studies.
作者
梁大伟
张漫
谭琳
王悦秋
LIANG Da-wei;ZHANG Man;TAN Lin;WANG Yue-qiu(Department of Pharmacy & Medical Laboratory,Ya’an Polytechnic College,Ya’an 625000,China)
出处
《食品与药品》
CAS
2019年第2期120-123,共4页
Food and Drug
基金
雅安市应用技术研究与开发项目(2017YYJSKF15)
关键词
氘代标记
吡罗昔康
合成
deuterium labeling
piroxicam
synthesis
