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5-硝基水杨醛硝化法的改进
The Reform of 5-Nitrosaicylaldehyde Nitrifying Means
【摘要】 探讨了以水杨醛为原料,混酸代替发烟硝酸为硝化剂制备5-硝基水杨醛的合成工艺,研究了混酸的用量、温度、溶剂和反应时间等条件对5-硝基水杨醛收率的影响.结果表明:在硝酸的用量是理论用量的1.25倍,浓硝酸与浓硫酸的物质的量比为1:2.5,在5~10℃反应3 h,然后升温到40℃充分反应2 h,5-硝基水杨醛的收率可达56.5%.
【Abstract】 The sysnthesis of 5-nitrosaicylaldehyde by nitration of salycyladehyde with mixed acid instead of fuming nitric acid was studied.The effects of the amount of mixed acid,temperature,solvents and the reaction time on the yield of 5-nitrosaicylaldehyde were also discussed.The best conditions were deduced as follows: 5-nitrosaicylaldehyde was synthesized from salicylicaldehyde and 68% nitric acid with 98% sulfuric acid(1:1.25:1.25×2.5 mol),the reaction mixture were maintained temperature below about 10 ℃ for 3 hours,then rise the temperature to about 40℃ for 2.5 hours so that it can reacted totally.Under this optimum conditions,the yield of 5-nitrosaicylaldehyde was exceeded 56.5%.The product has been determined by melting point method and characterized by infrared spectroscopy.
- 【文献出处】 湖南文理学院学报(自然科学版) ,Journal of Hunan University of Arts and Science(Natural Science Edition) , 编辑部邮箱 ,2006年01期
- 【分类号】O625.41
- 【被引频次】9
- 【下载频次】450