医药中间体4-[(4-甲基-1-哌嗪基)羰基]苯胺的合成研究

Synthesis of 4-[(4-Methyl-1-piperazinyl)carbonyl]Aniline as a Medicine Intermediate

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%。

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.