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 Pd-organophosphine
王振州 1竺来发 1尤瑶瑶 1吴曼 1曹金艳 1陈灿 1成鸿静1
作者信息
- 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;农用化学品湖南省重点实验室,湖南长沙 410014
- 折叠
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(K2CO3)∶n(复合催化剂)=1∶1.2∶1.2∶0.000 5,反应温度85 ℃,反应时间4 h,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.
Abstract
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(K2CO3)∶n(composite catalyst)=1∶1.2∶1.2∶0.000 5,the reaction temperature was 85 ℃,the reaction time was 4 h,the purity was 98.0％,and the yield 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Key words
2-amino-5-fluoro-3',4'-dichlorobiphenyl/Pd-organophosphine/Bixafen/Suzuki coupling reaction引用本文复制引用
出版年
2024
NETL
NSTL
万方数据