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对氯苯甲醛卤素交换氟化新工艺研究
Study of halogen-exchange fluorination of 4-chlorobenzaldehyde
【摘要】 研究了以对氯苯甲醛(PCAD)和无水KF为原料合成对氟苯甲醛(PFAD)的氟化反应。在溶剂选择、催化机理、工艺优化、动力学以及副反应研究等方面进行了相关探讨。在以硝基苯为溶剂,n(KF)∶n(PCAD)∶n(Ph4PBr)∶n(催化剂A)=3∶1∶0.1∶0.05、反应温度210℃、反应时间8 h的最佳工艺条件下,产品对氟苯甲醛的收率可达80.9%,纯度99.5%以上。
【Abstract】 The fluorination of 4-chlorobenzaldehyde was studied in solvents using spray-dried KF as fluorinating agent.In addition,the factors influencing the yield were discussed on solvents selecting,catalytic mechanism,process optimizing,dynamical equation and by-reaction control.Under the optimum reaction conditions as n(KF)∶n(PCAD)∶n(Ph4PBr)∶n(Cat.A)=3∶1∶0.1∶0.05,reacting at 210℃ for 8 h with nitrobenzene as a solvent,the yield of 4-fluorobenzaldehyde can reach 80.9% with purity of higher than 99.5%.
【关键词】 对氯苯甲醛;
对氟苯甲醛;
卤素交换氟化;
相转移催化;
防脱卤剂;
【Key words】 4-chlorobenzaldehyde; 4-fluorobenzaldehyde; halogen-exchange fluorination; phase transfer catalysis; anti-dehalogenating agent;
【Key words】 4-chlorobenzaldehyde; 4-fluorobenzaldehyde; halogen-exchange fluorination; phase transfer catalysis; anti-dehalogenating agent;
【基金】 江苏省科技攻关项目(BE2004045)
- 【文献出处】 现代化工 ,Modern Chemical Industry , 编辑部邮箱 ,2006年S1期
- 【分类号】TQ244.4
- 【被引频次】4
- 【下载频次】205