3-氯-5-(三氟甲基)-2-乙胺基吡啶的合成

Synthesis of 3-Chloro-5-(trifluoromethy1)-2-ethylaminopyridine

以2,3-二氯-5-三氟甲基吡啶为起始原料,先经亲核取代和脱羧两步反应"一锅法"合成了3-氯-5-(三氟甲基)-2-乙腈基吡啶,然后再经加氢还原和酰胺水解反应合成了3-氯-5-(三氟甲基)-2-乙胺基吡啶。3-氯-5-(三氟甲基)-2-乙胺基吡啶的外标含量为98. 6%,反应总收率为68. 8%,比文献[10]报道的收率高7%,并实现了N,N-二甲基乙酰胺的回收和重复利用。

3-Chloro-5-( trifluoromethy1)-2-ethylaminopyridine was synthesized by a four-step reaction of nucleophilic substitution reaction,decarboxylation,hydrogenation and hydrolysis with 2,3-dichloro-5-( trifluoromethyl)-pyridine as the starting material. And the nucleophilic substitution reaction and decarboxylation were processed by one-pot. The total yield is 68. 8% with the product purity of 98. 6%,7% higher than that in literature[10],and the recovery and reuse of N,N-dimethyl-acetamide were achieved.