Pd-有机膦催化Suzuki偶联合成2-氨基-5-氟-3',4'-二氯联苯  

Synthesis of 2-Amino-5-fluoro-3',4'-dichlorobiphenyl by Suzuki Coupling Catalyzed by Pdorganophosphine

作　　者：王振州 竺来发 尤瑶瑶 吴曼 曹金艳 陈灿 成鸿静 WANG Zhen-zhou;ZHU Lai-fa;YOU Yao-yao;WU Man;CAO Jin-yan;CHEN Can;CHENG Hongjing(National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry Co.,Ltd.,Changsha 410014,China;Agrochemical Key Laboratory of Hunan Province,Changsha 410014,China)

机构地区：[1]湖南化工研究院有限公司国家农药创制工程技术研究中心,湖南长沙410014 [2]农用化学品湖南省重点实验室,湖南长沙410014

出　　处：《精细化工中间体》2024年第6期13-16,共4页Fine Chemical Intermediates

基　　金：湖南省企业科技创新创业团队项目(湖南海利新材料科技创新创业团队)。

摘　　要：以3,4-二氯苯硼酸和2-溴-4-氟苯胺为原料,在碱性条件下使用Pd-有机膦复合催化剂进行Suzuki偶联反应,经分液、减压浓缩得到2-氨基-5-氟-3',4'-二氯联苯。通过对不同反应条件进行优化,获得优化条件为:以甲苯和水为混合溶剂,n(2-溴-4-氟苯胺)∶n(3,4-二氯苯硼酸)∶n(K_(2)CO_(3))∶n(复合催化剂)=1∶1.2∶1.2∶0.0005,反应温度85℃,反应时间4h,产物纯度98.0%,收率大于97.0%。该方法催化剂用量少、工艺简单、产品收率高,符合绿色化学生产理念,具有工业化前景。Using 3,4-dichlorophenylboronic acid and 2-bromo-4-fluoroaniline as raw materials,a Pd-organophosphine composite catalyst was used for Suzuki coupling reaction under alkaline conditions,and 2-amino-5-fluoro-3',4'-dichlorobiphenyl was obtained after separation and reduced pressure concentration.The results under different reaction conditions were analyzed,and the optimized conditions were:toluene and water as mixed solvents,n(2-bromo-4-fluoroaniline):n(3,4-dichlorophenylboronic acid):n(K_(2)CO_(3)):n(composite catalyst)=1:1.2:1.2:0.0005,the reaction temperature was 85℃,thereactiontimewas4h,thepurity was98.0%,and theyield was greater than 97.0%.The method requires less catalyst,has a simple process,and has a high product yield.It conforms to the concept of green chemical production and has industrial prospects.

关 键 词：2-氨基-5-氟-3' 4'-二氯联苯 Pd-有机膦 联苯吡菌胺 Suzuki偶联反应 

分 类 号：Q426.6[生物学—神经生物学] O643.36[生物学—生理学] TQ455.44[理学—物理化学]