氟吡菌酰胺的合成工艺优化

Optimized Process for the Preparation of Fluopyram

[目的]从合成条件和分离方法2方面对氟吡菌酰胺的合成工艺进行优化。[方法]2,3-二氯-5-三氟甲基吡啶与氰乙酸甲酯采用缩合反应和脱酯基反应"一锅法"的方法得到2-腈乙基-3-氯-5-三氟甲基吡啶,其在Raney-Ni催化下加氢还原得到2-乙胺基-3-氯-5-三氟甲基吡啶。2-乙胺基-3-氯-5-三氟甲基吡啶与邻三氟甲基苯甲酰氯反应得到氟吡菌酰胺。[结果]氟吡菌酰胺的总收率为51.4%,纯度98%。[结论]本工艺关键步骤采用2步反应一锅法的方法,操作简单,适合规模化生产。

[Aims] This study aims to optimize the process for the preparation of fluopyram on the synthesis conditions and separation method. [Methods] 3-chloro-5-（trifluoromethyl）-2-（2-cyanomethyl）pyridine was obtained from the condensation of 2, 3-dichloro-5-（ trifluoromethyl） pyridine with methyl cyanoa-cetate and demethoxycarbonylation by one-pot method, which is catalytically hydrogenated by Raney nickel to give3-chloro-5-（ trifluoromethyl）-2-（ 2-aminoethyl） pyridine. Finally, 2-ethyl-amino-3-chloro-5-trifluoromethylpyridine was reacted with o-trifluoromethylbenzoyl chloride to obtain fluopyram. [Results] The total yield was 51.4% and the purity was 98%. [Conclusions] The key steps of the process were to use one-pot method, which was simple and suitable for large-scale production.