摘要
在冰醋酸催化的无溶剂条件下,于室温合成了氘代PMP及其类似物——1-五氘代苯基-3-甲基-5-吡唑啉酮(d5-PMP),1,3-二苯基-5-吡唑啉酮(DPP)和1-(4-异丙苯基)-3-甲基-5-吡唑啉酮(PPMP),其中d5-PMP和PPMP为新化合物,其结构经UV,1H NMR,13C NMR,MS及元素分析表征。通过ESI-MS对d5-PMP,DPP及PPMP与乳糖的衍生化性能进行了初步研究。结果表明,d5-PMP和乳糖的反应活性最高,衍生物以双分子标记物为主,衍生化性能与d0-PMP相当;DPP的反应活性最低,单分子和双分子标记物产率相当,不适用于糖类物质的衍生化分析;PPMP的反应活性仅次于d5-PMP或d0-PMP,生成稳定性较好的单分子标记物的倾向较大,优化衍生条件使其定量进行可用于糖类物质分析。
Three 1,3-substitutive pyrazolones reagents, 1- （pentadeuterium） phenyl-3-methyl-5-pyrazolone （ ds-PMP ）, 1,3-diphenyl-5-pyrazolone （ DPP ） and 1- （ 4-isopropyl ） phenyl-3-methyl-5-pyrazolone （ PPMP）, were synthesized under the conditions of using glacial acetic acid as the catalyst in solvent- free state at room temperature, d5-PMP and PPMP were new compounds. The structures were characterized by UV, 1H NMR, 13C NMR, MS and elemental analysis. The reaction activities of d5-PMP, DPP and PPMP with lactose were investigated by ESI-MS. The results indicated that d5-PMP exhibi- ted the highest reaction activity and obtained mainly dimolecular derivatives, DPP exhibited the lowest reaction activity and failed to as saccharide＇ s derivatization reagent, and PPMP exhibited the second reaction activity following d5-PMP（ or d0-PMP） and trended to generate unimoleeule derivatives with better stability than dimolecular derivatives, no PPMP losing happened, and can be used to analyze the saccharides if the quantitative dcrivatization condition is optimized.
出处
《合成化学》
CAS
CSCD
北大核心
2013年第3期262-266,293,共6页
Chinese Journal of Synthetic Chemistry
基金
国家自然科学基金资助项目(31170773)
陕西省科技厅自然科学基金资助项目(2012JQ2014)
陕西省教育厅自然科学基金资助项目(2013JK0670)
咸阳师范学院科研基金资助项目(11XSYK103)
关键词
吡唑啉酮
酸催化
乳糖
合成
衍生化性能
pyrazolone
acid catalysis
lactose
synthesis
derivatization performance
