4-溴-2-氟联苯的“一锅法”合成

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16h。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。

Synthesis of 4-Bromo-2-fluorobiphenyl by One Pot Method

4-Bromo-2-fluorobiphenyl was synthesized by one pot method using 4-bromo2-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 16h.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.