对氟苯胺的合成  

Synthesis of 4-Fluoroaniline

作　　者：徐德忠 

机构地区：[1]浙江富盛控股集团有限公司研发中心,浙江常山324202

出　　处：《化工生产与技术》2007年第1期4-6,共3页Chemical Production and Technology

摘　　要：以对氯硝基苯和活性氟化钾等为原料,经二步法合成了对氟苯胺。实验结果表明,氟化反应的最佳条件为:二甲基甲酰胺为溶剂、复合季铵盐为催化剂,n(对硝基氯苯):n(KF)=1:1.2,m(催化剂):m(对硝基氯苯)=4%,m(DMF):m(对硝基氯苯)=1:1,于155～160℃下反应18h;还原反应在甲醇中进行,以阮内镍为催化剂;粗产品加入抗氧剂,减压条件下简单蒸馏得高品位的对氟苯胺。所得对氟苯胺纯度99.5%以上,总收率89.3%,在室内敞口放置2个月未见明显变色,具工业价值。4-Fluoroaniline is synthesized in two steps from p-nitrochlorobenzene and active potassium fluoride.Optimum conditions are as follows:DMF is used as solvent,compound quaternary ammonium salt as catalyst,n(p-nitrochloro benzene):n(KF)=1:1.2,m(catalyst):m(p-nitrochloro benzene)=4%,m(DMF):m(p-nitrochloro benzene)=1:1,and reacted under 155～160 ℃ for 18 h;reduction reaction is carried out in methanol with Raney nickel,which is used as catalyst;the raw product is added an antioxidant,and distilled simply under reduced pressure to obtain 4-fluoroaniline with excellence quality,purity is over 99.5%,total yield is 89.3%.2 moths later it is stored uncorked in room,no color change is obvioused,which shows this process has some value in industry.

关 键 词：对氟苯胺 活性氟化钾 对氯硝基苯 对氟硝基苯 复合季铵盐 催化加氢 

分 类 号：TQ246[化学工程—有机化工]