2-氯-5-氨甲基吡啶的合成研究

Synthesis of 2-chloro-5-(aminomethyl) Pyridine

根据Delépine伯胺制备方法,以2-氯-5-氯甲基吡啶和六次甲基四胺为原料,实验室制备2-氯-5-氨甲基吡啶。考察了反应过程溶剂的种类及数量、酸碱用量、原料配比对反应的影响,发现以乙腈作溶剂,在n(C6H5NCl2):n[(CH2)6N4]=1∶1.1,n((CH2)6N4):n(HCl):n(NaOH)=1∶8∶8,溶剂量100 mL,反应温度为溶剂沸点的反应条件下,2-氯-5-氨甲基吡啶总收率>89%。产品经NMR分析,结构正确。

Based on Delepine,2 - ehloro - 5 - ehloromethylpyridine was treated with tetramine to afford 2 - ehloro - 5 - （aminomethyl） pyridine. Efflect of solvent variety and quantity were studied. Acid quantity and ratio of raw material were studied too.The optimum reaetion condition： n（C6H5NCl2）： n[ （CH2）6N4]1： 1.1, n[ （CH2）6N4] ： n（HCl） ： n（NaOH） = 1： 8 ： 8, aeetonitrile 100 mL, 82 ℃ with the yield 〉 89 %. The final products were characterized by HNMR which show that resultants are the objeetive products.