| 5-溴烟腈的合成及表征 |
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| 引用本文： | 黄凤远,张福辰,陈启凡.5-溴烟腈的合成及表征[J].辽东学院学报(自然科学版),2010,17(1):5-7. |
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| 作者姓名： | 黄凤远 张福辰 陈启凡 |
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| 作者单位： | 辽东学院化工与材料学院,辽宁,丹东,118003;辽东学院实验中心,辽宁,丹东,118003 |
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| 摘 要： | 以5-溴烟酸(Ⅰ)为起始原料,经SOCl2氯化制备5-溴烟酰氯(Ⅱ),收率为90%;Ⅱ与氨水在冰水浴(0~10℃)下反应合成了5-溴-烟酰胺(Ⅲ),收率为79%;以三氯氧磷为氧化剂,在110℃回流反应,将Ⅲ氧化制备成目标产物5-溴烟腈(Ⅳ),收率为68%。以此方法制备5-溴烟腈(Ⅳ)总收率可达到48%。中间产物和目标产物通过傅里叶变换红外光谱和核磁共振氢谱进行了结构确证。
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| 关 键 词： | 5-溴烟腈 5-溴烟酸 5-溴烟酰胺 合成 |
Synthesis and Characteristics of 5-Bromo-nicotinonitrile |
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| HUANG Feng-yuan,ZHANG Fu-chen,CHEN Qi-fan.Synthesis and Characteristics of 5-Bromo-nicotinonitrile[J].Journal of Liaodong University：Natural Sciences,2010,17(1):5-7. |
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| Authors: | HUANG Feng-yuan ZHANG Fu-chen CHEN Qi-fan |
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| Affiliation: | HUANG Feng-yuan1,ZHANG Fu-chen1,CHEN Qi-fan2(1.College of Chemical Engineering and Material Science,Eastern Liaoning University,Dandong 118003,China,2.Experiment Center,China) |
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| Abstract: | Firstly,5-Bromo-nicotinic acid,the initial reactant,was chlorinated with SOCl2,thus preparing 5-Bromo-nicotinate with 90% yield;secondly,5-Bromo-nicotinamide was prepared from the reaction of 5-Bromo-nicotinate with ammonium aqueous at 0～10 ℃ with 79% yield;thirdly,with POCl3 as the oxidant,5-Bromo-nicotinonitrile was obtained by 5-Bromo-nicotinamide via a reflux reaction at 110 ℃ with 68% yield.The total yield was more than 48% by this method.The structures of intermediates and target product were characterized with FT-IR and 1H NMR. |
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| Keywords: | 5-Bromo-nicotinonitrile 5-Bromo-nicotinic acid 5-Bromo-nicotinamide synthesis |
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