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%.
The sysnthcsis 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.
出处
《湖南文理学院学报（自然科学版）》
CAS
2006年第1期31-32,52,共3页
Journal of Hunan University of Arts and Science(Science and Technology)
关键词
5-硝基水杨醛
混酸
硝化
5-nitrosaicylaldehyde, mixed acid, nitrifying reaction
