| 第 51 卷第 2 期 |  | Vol. 51 No. 2 | | 2021 年 4 月 | Apr 2021 |
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所屬欄目：農藥及中間體
N-異十三烷基-2，6-二甲基嗎啉的工藝改進(jìn) |
| 黃 勇，湯 燕，楊?lèi)?ài)華，白俊華，吳世剛*
（合肥億帆生物制藥有限公司，安徽 合肥 230000） |
| 摘 要：以2，6-二甲基嗎啉和異構十三醇為原料，合成了N-異十三烷基-2，6-二甲基嗎啉，并優(yōu)化了反應條件。優(yōu)化條件為：n（異構十三醇）∶n（2，6-二甲基嗎啉）=1.2∶1.0，反應溫度260~280 ℃，2，6-二甲基嗎啉滴加時(shí)間為8~10 h，優(yōu)化條件下，N-異十三烷基2，6-二甲基嗎啉收率達86.9%，純度96%以上，產(chǎn)品結構經(jīng)紅外和質(zhì)譜確證。該工藝具有成本低、工藝流程短、操作簡(jiǎn)便、收率高等優(yōu)勢，宜于產(chǎn)業(yè)化。 |
| 關(guān)鍵詞：十三醇；2，6-二甲基嗎啉；一步法 |
| 中圖分類(lèi)號：S482.2 文獻標識碼：A 文章編號：1009-9212（2021）02-0027-02 |
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| 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 |
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作者簡(jiǎn)介：黃 勇（1973—），男，湖南南通人，工程師，主要從事農藥及醫藥產(chǎn)品的開(kāi)發(fā)研究工作。
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聯(lián) 系 人：吳世剛，執業(yè)藥師，碩士，主要從事原料藥的研發(fā)和產(chǎn)業(yè)化轉化（E-mail：wushigang@yifanyy.com）。
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收稿日期：2021-04-05
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