全文下载: 2012010021
唐林生, 毕凤云, 刘全美, 李永强
(青岛科技大学 化工学院, 山东 青岛 266042)
摘要:以4-溴-2-氟苯胺溴酸盐为原料,经重氮化、偶联反应,采用“一锅法”合成了4-溴-2-氟联苯,考察了各因素对反应的影响。结果表明,最佳反应条件是n(4-溴-2-氟苯胺溴酸盐)∶n(亚硝酸钠)∶n(复合酸)∶n(氯化亚铜)=1∶1.180∶1.36∶0.059,反应温度为40 ℃,反应时间为16 h。在以上条件下,产品收率为63.85%。该方法工艺流程简单,反应条件温和,采用复合酸代替三氯乙酸,产品收率略低,但酸性试剂的成本降低了95%以上。
关键词: 4-溴-2-氟苯胺; 4-溴-2-氟联苯; “一锅法”合成
中图分类号: R 914文献标志码: A
Synthesis of 4-Bromo-2-fluorobiphenyl by One Pot Method
TANG Lin-sheng, BI Feng-yun, LIU Quan-mei, LI Yong-qiang
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042,Chiina)
Abstract:4-Bromo-2-fluorobiphenyl was synthesized by one pot method using 4-bromo-2-fluoroaniline bromate as starting material through diazotization and coupling reaction. The effects of various condition parameters on reaction results were examined. The optimum reaction conditions were n(4-bromo-2-fluoroaniline bromate)∶n(sodium nitrite)∶n(composite acid)∶n(cuprous chloride)=1∶1.180∶1.36∶0.059,reaction temperature 40℃, and reaction time being 16 h. Under above conditions, the yield of product was 63.85%. The cost of acidic reagent could be reduced as much as 95% by using composite acid instead of trichloroacetic acid, although the yield of product was slightly decreased.
Key words: 4-bromo-2-fluoroaniline; 4-bromo-2-fluorobiphenyl; one pot method
收稿日期:2011-03-18
作者简介:唐林生(1962—),男,教授.