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改进Duff反应合成5-硝基水杨醛
Improves the Method of the Duff Response to Prepare 5-nitrosaicyl Aldehyde
【摘要】 用多聚磷酸改进Duff反应合成了5-硝基水杨醛,探讨了温度、时间、反应物用量等因素对5-硝基水杨醛产率的影响。结果表明较佳反应条件是:在对硝基苯酚为3.5 g的情况下,75%的多聚磷酸用量为30 mL,n(六亚甲基四胺)∶n(对硝基苯酚)=2∶1,反应时间为3.0 h,反应温度105℃,5-硝基水杨醛的产率可达68.1%。并对产品进行了红外检测,符合文献值的要求。
【Abstract】 Synthesis of 5-nitrosaicylaldehyde was studied by the improved method of the Duff response with polyphosphoric acid.The effects of reaction time and temperature etc on the yield of 5-nitrosaicylaldehyde were also investigated.The studies showed that the optimum conditions of the reaction were the amount of the 75% gathers the phosphoric acid 30 mL,the mole ratio ofhexamethylene tetramine to nitrophenol was 2∶1,the reaction time was about 3.0 hours,the reaction temperature was about 105℃.Under the optimum conditions,the highest yield of 5-nitrosaicylaldehyde reached 68.1%.The product was determined by infrared spectroscopy.
【Key words】 5-nitrosaicy|aldehyde; polyphosphoric; acid; formylation; Duff; reaction;
- 【文献出处】 化工时刊 ,Chemical Industry Times , 编辑部邮箱 ,2006年12期
- 【分类号】TQ244.1
- 【被引频次】9
- 【下载频次】741