On the basis of the Zaleplon structure, novel pyrazolo[l,5-a]pyrimidines were designed and prepared for studies on their hypnotic activity. This paper reported the synthesis of twelve new 5-methyl-7-substituted-pyrazo...On the basis of the Zaleplon structure, novel pyrazolo[l,5-a]pyrimidines were designed and prepared for studies on their hypnotic activity. This paper reported the synthesis of twelve new 5-methyl-7-substituted-pyrazolo[1,5-a]pyrimidine-3-carbonitrile derivatives by using simple starting materials such as propane dinitrile and triethyl orthoformate. The structures of the derived target compounds were confirmed by their IR and 1H-NMR spectroscopic data. The preliminary pharmacological evaluations indicated that some compounds showed hypnotic activity, while derivative 1c was the most polent one.展开更多
文摘On the basis of the Zaleplon structure, novel pyrazolo[l,5-a]pyrimidines were designed and prepared for studies on their hypnotic activity. This paper reported the synthesis of twelve new 5-methyl-7-substituted-pyrazolo[1,5-a]pyrimidine-3-carbonitrile derivatives by using simple starting materials such as propane dinitrile and triethyl orthoformate. The structures of the derived target compounds were confirmed by their IR and 1H-NMR spectroscopic data. The preliminary pharmacological evaluations indicated that some compounds showed hypnotic activity, while derivative 1c was the most polent one.
文摘目的：建立中成药及保健品中添加镇静安神类化学药品的HPLC-DAD及HPLC-MS/MS分析方法,建立HPLC-DAD数据库及二级质谱库,并应用分析。方法：HPLC-DAD法采用Agilent ZORBAX Eclipse Plus C8（4.6 mm×150 mm,5μm）色谱柱,0.02 mmol·L^-1磷酸二氢钾-甲醇（95∶5）为流动相,流速1.0 m L·min^-1;HPLC-MS/MS法采用Shim-Pack VP-ODS（150 mm×2.0 mm,5μm）色谱柱,0.1%甲酸-乙腈为流动相,梯度洗脱,流速0.3 m L·min^-1,质谱检测器以正离子和MRM方式进行检测。样品以甲醇为溶剂,超声提取。结果：HPLC-DAD法采用有效相对保留时间和紫外光谱相似度双指标进行定性准确可靠,相对校正因子法回收率98%-105%。优化HPLC-MS/MS条件,确定了定性离子及建立质谱库的最佳质谱条件。结论：该法快速准确,适用于中成药及保健品中非法添加镇静安神类化学药的质量监控,为替代对照品法及二级质谱库在此类研究中提供依据。
