摘要
[目的]改进含氟中间体3-氟苯甲酸的合成方法。[方法]以3-氨基苯甲酸为起始原料,在氟化氢吡啶试剂中进行重氮化和氟化反应合成3-氟苯甲酸,并经正交试验优化得到最佳条件。[结果]氟化氢吡啶试剂浓度为70%,3-氨基苯甲酸、NaNO_2和氟化氢吡啶投料摩尔比为1∶1∶50,收率为96.90%,纯度为99.09%。[结论]利用氟化氢吡啶试剂合成3-氟苯甲酸具有反应条件温和、收率高、后处理方便等优点,实用性强。
[Aims] Improvement of the synthesis of fluorine-contained intermediate 3-fluorobenzoic acid. [Methods] 3- Fluorobenzoic acid was synthesized from 3-aminobenzoic acid by diazotization and fluorination in the reagent of hydrogen fluoride-pyridine. An optimized reaction condition was obtained through orthogonal experiment [Results]With 70% hydrogen fluoride-pyridine reagent and a mole ratio of 3-aminobenzoic acid, NaNO2 to HF as 1：1：50, the 3-fluorobenzoic acid was yield in 96.90% with purity of 99.09%. [Conclusions] The synthesis of 3-fluorobenzoic acid using hydrogen fluoride-pyridine is a practical method with advantages of mild reaction conditions, high yield and convenient post-treatment.
出处
《农药》
CAS
CSCD
北大核心
2018年第2期90-92,共3页
Agrochemicals
关键词
3-氟苯甲酸
氟化氢吡啶
重氮化
3-fluorobenzoic acid
hydrogen fluoride-pyridine
diazotization
