| 第 51 卷第 2 期 |  | Vol. 51 No. 2 | | 2021 年 4 月 | Apr 2021 |
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所属栏目：医药及中间体
医药中间体4-［（4-甲基-1-哌嗪基）羰基］苯胺的合成研究 |
| 姜晓晔，张 焕，雷 雪，黎七雄*
（武汉城市学院，湖北 武汉 430083） |
| 摘 要：以氮甲基哌嗪为原料，经对硝基苯甲酰氯酰化和硝基Fe粉还原两步反应合成了医药中间体4-［（4-甲基-1-哌嗪基）羰基］苯胺，并通过单因素实验优化合成工艺。酰化反应：溶剂为CH2Cl2，缚酸剂为K2CO3，收率95.67%。还原反应用NH4Cl活化后的Fe粉为还原剂，投料比为n（4-［（4-甲基-1-哌嗪基）羰基］硝基苯）∶n（铁粉）∶n（NH4Cl）=1∶4∶4，收率90.14%。总收率82.97%。 |
| 关键词：4-［（4-甲基-1-哌嗪基）羰基］苯胺；医药中间体；单因素实验 |
| 中图分类号：R97 文献标识码：A 文章编号：1009-9212（2021）02-0038-04 |
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| Synthesis of 4-[(4-Methyl-1-piperazinyl)carbonyl] Aniline as a Medicine Intermediate |
| IANG Xiao-ye, ZHANG Huan, LEI Xue, LI Qi-xiong*
(Wuhan City College, Wuhan 430083, China) |
| Abstract：4-[(4-Methyl-1-piperazinyl)carbonyl] aniline was synthesized through a two-step reaction including acylation and reductionby one-factor experiment to determine the most excellent synthesis process using nitrogen-methyl piperazine as the raw material. The results showed that: in acylation reaction, N-methyl piperazine and p-nitrobenzoyl chloride were reacted to prepare 4-[(4-methyl-1-piperazinyl) carbonyl] nitrobenzenethe;a yield of 95.67% was achieved using CH2Cl2 as the solvent and K2CO3 as the deacid reagent.While in thereduction reaction,the reduction4-[(4-Methyl-1-piperazinyl)carbonyl]nitrobenzene by Fe was actived by NH4Cl to preparation 4-[(4-methyl-1-piperazinyl) carbonyl] aniline;a yield of 90.14% was achieved when.the ratio of 4-[(4-methyl-1-piperazinyl) carbonyl] nitrobenzene: iron: NH4Cl was 1∶4∶4. A total yield of 82.97% was achieved. |
| Key words：4-[(4-methyl-1-piperazinyl) carbonyl] aniline; medicine intermediate; one-factor experiment |
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作者简介：姜晓晔（1987—），女，湖北武汉人，硕士，研究方向：药物合成反应（E-mail：511811879@qq.com）。
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联 系 人：黎七雄，教授，研究方向：药学（E-mail：1015563065@qq.com）。
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收稿日期：2021-04-28
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