| 6-硝基喹哪啶的合成工艺改进 |
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| 引用本文： | 陈玉风,严正权,徐洪耀.6-硝基喹哪啶的合成工艺改进[J].合成化学,2010,18(2). |
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| 作者姓名： | 陈玉风 严正权 徐洪耀 |
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| 作者单位： | 东华大学,材料科学与工程学院,纤维材料改性国家重点实验室,上海,201620 |
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| 基金项目： | 国家自然科学基金，教育部博士培养基金 |
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| 摘 要： | 以I2/KI为氧化剂,甲苯为乳化剂,对硝基苯胺(2)和巴豆醛(3)经环合反应合成了6-硝基喹哪啶(1)。最佳反应条件为:28.92 mmol,甲苯10 mL,混酸45.5 mLV(AcOH)∶V(HCl)=1∶90],n(2)∶n(I2/KI)=1∶1,于100℃反应4 h,收率达93.1%。1的结构经1HNMR,IR和元素分析表征。
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| 关 键 词： | 6-硝基喹哪啶 Skraup-Doebner-Von Miller反应 工艺改进 合成 |
Process Improvement on the Synthesis of 6-Nitrylquinaldine |
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| CHEN Yu-feng,YAN Zheng-quan,XU Hong-yao.Process Improvement on the Synthesis of 6-Nitrylquinaldine[J].Chinese Journal of Synthetic Chemistry,2010,18(2). |
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| Authors: | CHEN Yu-feng YAN Zheng-quan XU Hong-yao |
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| Abstract: | 6-Nitrylquinaldine(1) was synthesized by cyclization of p-nitroaniline(2) with crotonaldehyde(3) using I_2/KI as the oxidant and toluene as the emulsifier. The structure was characterized by ~1H NMR, IR and elemental analysis. The optimum reaction conditions at 100 ℃ for 4 h were as follows: 2 was 8.92 mmol;toluene was 10 mL;mixed acidV(AcOH) ∶ V(HCl)＝1 ∶ 90] was 45.5 mL;n(2) ∶ n(I_2/KI)＝1 ∶ 1. The yield of 1 can reach 93.1% under the conditions. |
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| Keywords: | 6-nitrylquinaldine Skraup-Doebner-Von Miller Reaction process improvement synthesis |
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