【摘要】 目的优化1-（4-氨苯基）-3-吗啉-5,6-二氢吡啶-2（1H）-酮的合成工艺。方法以对硝基苯胺为原料,经酰胺化、环合、双氯代、硝化还原等五步反应得到目标化合物。去除了环合催化剂氢化钠的使用,改进了反应缚酸剂,降低了中间体反应温度,探究了反应最优配比条件,并对各步反应后处理进行了工艺条件优化。结果目标化合物经¹H NMR,¹³C NMR谱确认,反应总收率达65.4%。结论优化后的工艺操作简便,条件温和可控,溶剂易于回收利用,污染小,更加利于工业化的生产。更多还原

【Abstract】 Objective To optimize the synthesis process of 1-（4-aminophenyl）-5,6-dihydro-3-（4-orpholinyl）-2（1H）-pyridinone.Methods Using p-nitroaniline as the raw material,the target compound was obtained by amidation,cyclization,chlorination,nitration and reduction reactions.The sodium hydride catalyst for cyclization was taken out in the reaction,the reaction acid binding agent was improved,the reaction temperature of intermediate was reduced,the optimal ratio and reaction ratio condition were investigated,and the post-processing conditions were optimized for each reaction.Results The target compound was confirmed by ¹H NMR and ¹³C NMR data,and the total yield was 65.4%.Conclusion The optimized process is simple to operate,mild and controllable,and the solvent is easy to recycle,low-polluting and more conducive to industrial production.更多还原