N-甲基哌啶的合成方法研究
Study on the Synthesis Method of N-Methylpiperidine
何小强 1郝磊 1向龙 1李倩文1
作者信息
- 1. 重庆华歌生物化学有限公司,重庆 404000
- 折叠
摘要
目的:建立N-甲基哌啶的合成方法并考察合成条件对其含量的影响.方法:以哌啶、甲醛为原料,以甲酸钠和甲酸为还原剂,经烷基化得N-甲基哌啶溶液,再经环己烷萃取及精馏得N-甲基哌啶.结果:在哌啶、还原剂组分、甲醛投料摩尔比为1∶1.2∶1.2,滴加速度为3.33 mL/min,滴加时间为 60 min,反应温度为 80℃的最佳条件下反应 3h,得到的N-甲基哌啶含量为99.1%;经环己烷萃取,精馏后,含量为 99.5%,收率为 98.7%.结论:该方法反应条件温和、产品纯度高、工艺简单、易实现工业化.
Abstract
Objective:To establish a synthesis method of N-methylpiperidine and to investigate the effect of synthesis conditions on its content.Methods:Using piperidine and formaldehyde as raw materials,sodium formate and formic acid as reducing agents,N-methylpiperidine solution was obtained by alkylation,and then N-methylpiperidine was obtained by cyclohexane extraction and rectification.Results:The N-methylpiperidine content was 99.1%under the optimal conditions of 1∶1.2∶1.2,droplet acceleration of 3.33 mL/min,dropping time of 60 min and reaction temperature of 80℃for 3 h,and the content of N-methylpiperidine was 99.1%,and the content was 99.5%and the yield was 98.7%after cyclohexane extraction and distillation.Conclusion:The reaction conditions of this method are mild,the product purity is high,the process is simple,and it is easy to realize industrialization.
关键词
N-甲基哌啶/烷基化反应/环己烷/合成/萃取Key words
N-methylpiperidine/alkylation/cyclohexane/synthesis/extraction引用本文复制引用
出版年
2024
NETL
NSTL
万方数据