Fe/Fe_2O_3催化氨解合成农药中间体5-甲基-3,4-二氢吡啶-2(1H)-酮

Synthesis of 5-Methyl-3,4-dihydro-2(1H)pyridone Catalyzed by Fe/Fe_2O_3

[目的]5-甲基-3,4二氢吡啶-2(1H)-酮是一种重要的化工中间体,其经氯化可生成2-氯-5-甲基吡啶和2,3-二氯-5-甲基吡啶,2者均是十分重要的农药和医药中间体。[方法]以3-甲基-2-(4-吗啉基)环丁酸甲酯为原料,Fe/Fe2O3为组合催化剂,通过加压氨解一步法合成5-甲基-3,4-二氢吡啶-2(1H)-酮,并对反应温度、时间、氨水浓度、原料配比和催化剂种类等因素进行研究,采用GC-MS和1H NMR表征产品结构。[结果]在最佳工艺条件下,5-甲基-3,4-二氢吡啶-2(1H)-酮的收率为80.63%,纯度为98.95%。[结论]该方法操作简单、安全、三废少、催化剂廉价易回收、产品收率高,适合工业化生产。

[Aims] 5-Methyl-3,4-dihydro-2（1H）pyridonc was an important chemical intermediate, which can be utilized for synthesis of 2-dichloro-5-methylpyfidine and 2,3-dichloro-5-methyipyridine by chlorination reaction. [Methods] It was synthesized from methyl 3-methyl-2-morpholinocyclobutane-l-carboxylate and ammonia in the presence of Fe/Fe2O3. The influences of synthesis technology were investigated, and the structure of the target was confirmed by GC-MS and 1H NMR. [Results] Under optimized condition, the yield and purity of 5-methyl-3,4-dihydro-2 （1H） pyridone was 80.63 and 99.53%, respectively. [Conclusions] This process has the advantages of simpleness, safety, low waste disposal, catalyst recycling, high yield and suitability for industrial production.