第 51 卷第 2 期 Vol. 51 No. 2 2021 年 4 月 Apr 2021

所属栏目：农药及中间体 N-异十三烷基-2，6-二甲基吗啉的工艺改进

黄 勇，汤 燕，杨爱华，白俊华，吴世刚* （合肥亿帆生物制药有限公司，安徽 合肥 230000）

摘　要：以2，6-二甲基吗啉和异构十三醇为原料，合成了N-异十三烷基-2，6-二甲基吗啉，并优化了反应条件。优化条件为：n（异构十三醇）∶n（2，6-二甲基吗啉）=1.2∶1.0，反应温度260~280 ℃，2，6-二甲基吗啉滴加时间为8~10 h，优化条件下，N-异十三烷基2，6-二甲基吗啉收率达86.9%，纯度96%以上，产品结构经红外和质谱确证。该工艺具有成本低、工艺流程短、操作简便、收率高等优势，宜于产业化。

关键词：十三醇；2，6-二甲基吗啉；一步法

中图分类号：S482.2　　文献标识码：A　　文章编号：1009-9212（2021）02-0027-02

Process Improvement of 2,6-Dimethy-N-tridecyl Morpholine

HUANG Yong, TANG Yan, YANG Ai-hua, BAI Jun-hua, WU Shi-gang* (Hefei Yifan Biopharmaceutical Co.,Ltd., Hefei 230000, China)

Abstract：The synthetic process of 2,6-dimethy-N-tridecyl morpholine was improved using 2,6-dimethylmorpholine and isotridecanol as raw materials. Process conditions include the ratio of raw materials, reaction temperature and dropping time of 2,6-dimethylmorpholine were optimized. The optimized conditions was obtain as following: n(isomeric tridecanol)∶n(2,6-dimethylmorpholine) was of 1.2∶1.0, the reaction temperature was of 260~280 ℃, and the 2,6-dimethylmorpholine dropping time was of 8~10 h. Under these conditions, the yield and purity of n-isotridecyl 2,6-dimethylmorpholine were 86.9% and 96% respectively. The product structure was confirmed by IR and MS. The process has the advantages including low cost, short process flow, less investment, simple operation, high yield and industrialization.

Key words：tridecyl alcohol; 2,6-dimethylmorpholine; one-step method

作者简介：黄 勇（1973—），男，湖南南通人，工程师，主要从事农药及医药产品的开发研究工作。

联 系 人：吴世刚，执业药师，硕士，主要从事原料药的研发和产业化转化（E-mail：wushigang@yifanyy.com）。

收稿日期：2021-04-05