2-氯-N-(2-氯-4-甲基-3-吡啶基)-3-吡啶甲酰胺合成工艺改进

Improvement in Synthesis of 2-chloro-N-(2-chloro-4-methylpyridin-3-yl)pyridine-3-carboxamide

介绍了以4-甲基-3-氨基-2-氯吡啶(CAPIC)和2-氯烟酸合成2-氯-N-(2-氯-4-甲基-3-吡啶基)-3-吡啶甲酰胺的方法,并选择出了最优惠条件,反应最佳投料比为n(4-甲基-3-氨基-2-氯吡啶)∶n(2-氯烟酸)∶n(POCl3)∶n(Et3N)=1∶1∶1∶1.1,反应温度81℃,反应时间3.5 h,产品收率90.3%,纯度为99.5%。

2-Chloro-N-（2-chloro-4-methylpyridin-3-yl） pyridine-3-carboxamide was synthesized by the re- action of 2-chloro-3-aminO-4-methylpyridine （CAPIC） and 2-chloropyridine-3-carboxylic acid, and the optimal reaction conditions were investigated, the reactants molar ratio of [ 2-chloro-3-amino-4-methylpyr- idine： 2-chlorooctanic acid： POCI3： Et3N] was 1： 1： 1： 1.1, the reaction temperature 81 .9 C, and adding time of 3.5 h provided the best result. The yield and purity of the target product was 90. 3% and 99. 5%, respectively.