| 气相色谱-质谱监测1-溴-2,4-二氟苯的合成条件、贡献及纯度 |
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| 引用本文： | 刘剑敏,李艳霞,郭平,叶发青. 气相色谱-质谱监测1-溴-2,4-二氟苯的合成条件、贡献及纯度[J]. 分析科学学报, 2009, 25(3) |
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| 作者姓名： | 刘剑敏 李艳霞 郭平 叶发青 |
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| 作者单位： | 1. 温州医学院药学院,浙江温州,325035
2. 温州医学院分析测试中心,浙江温州,325035 |
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| 基金项目： | 浙江省温州市科技计划项目 |
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| 摘 要： | 采用气相色谱-质谱（GC—MS）法对1，3-二氟苯溴化产物定性分析，采用了峰面积归一化法对产物进行定量分析，并通过正交设计结合多指标综合评价法优化合成条件。结果表明，通过GC—MS监测，对正交实验Z值结果分析得到最佳制备工艺：四氯化碳为溶剂，反应摩尔比（间二氟苯与液态溴）2：1，5℃下反应12h。产物纯度高于99．50％
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| 关 键 词： | 1-溴-2 4-二氟苯 气相色谱-质谱 正交设计 多指标综合评价 |
Monitoring of Preparation Condition of 1-Bromo-2,4-difluorobenzene by Gas Chromatography/Mass Spectrometer |
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| LIU Jian-min,LI Yan-xia,GUO Ping,YE Fa-qing. Monitoring of Preparation Condition of 1-Bromo-2,4-difluorobenzene by Gas Chromatography/Mass Spectrometer[J]. Journal of Analytical Science, 2009, 25(3) |
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| Authors: | LIU Jian-min LI Yan-xia GUO Ping YE Fa-qing |
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| Affiliation: | 1.Department of Pharmaceutical Chemistry of Wenzhou Medical College;Wenzhou 325035;2.Analytical and Testing Center of Wenzhou Medical College;Wenzhou 325035 |
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| Abstract: | The m-difluorobenzene was brominated, and the composition and structure of products were analyzed by Gas Chromatography/Mass Spectrometer(GC/MS). The optimum preparation conditions were selected with orthogonal design combined with multi-index test. According to Z-score result, the optimum conditions for preparation of 1-bromo-2, 4-difluorobenzene was: temperature at 5℃ and reaction time at 12 h. The results showed that the product purity prepared under the optimum conditions was higher than 99.50%. |
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| Keywords: | 1-Bromo-2,4-difluorobenzene GC-MS Orthogonal design Multi-index test |
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