三氟百菌清的小试合成工艺

Improved Synthesis of 5-Chloro-2,4,6-trifuoro-1,3-benzenedicarbonitrile

三氟百菌清(5-氯-2,4,6-三氟-1,3-苯二甲腈)具有广谱、高效的抑菌活性。为了将其研究开发为新的杀菌剂原药,对其合成方法和合成工艺进行改进研究,确定了最佳的反应条件,为将来工业化生产奠定基础。结果表明,最佳合成工艺为:0.4 mol百菌清,450 mLDMF,1.65 mol无水KF,0.4 mmol催化剂,112℃反应4 h得到粗品。粗品与1600 mL环己烷回流30 min,25℃冷却,结晶0.5 h,得到三氟百菌清的纯品。通过工艺改进,粗品含量可达81.7%,提纯后含量可达99.0%,最终产率达60.0%。

Synthesis of 5-chloro-2,4,6-trifuoro-1,3-benzenedicarbonitrile was improved, and the optimal condition was chosen. Result showed that the content of crude product could be reach 81.7% when 0.4 mol of chlorothalonil was mixed with 450 ml of DMF, 1.65 tool of potassium fluoride and 0.4 mmol of catalyst, and reacted at 112℃ for 4 h. The crude product was refluxed with 1.6 L of cyclohexane for 30 min and then crystallized for 0.5 h to produce f 5-chloro-2,4, 6-trifuoro-1,3-benzenedicarbonitrile with the purity of 99.0% and the yield of 60.0%.