| 第 52 卷第 4 期 |  | Vol. 52 No. 4 | | 2022 年 8 月 | Aug 2022 |
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所属栏目：农药及中间体
呋虫胺代谢物UF的合成研究 |
| 郭 会，陈武炼
（上海安谱实验科技股份有限公司，上海 201600） |
| 摘 要：研究了一种全新的呋虫胺代谢物UF的合成方法，即以N-甲基-1-咪唑甲酰胺和3-氨基甲基四氢呋喃为原料，在有机碱催化下室温反应得到呋虫胺代谢物UF。考察了反应的影响因素，确定了优化反应条件：n（N-甲基-1-咪唑甲酰胺）∶n（3-氨基甲基四氢呋喃）=1.0∶1.0，催化剂使用三乙胺或吡啶，n（催化剂）∶n（N-甲基-1-咪唑甲酰胺）=1.1∶1.0，反应温度为25 ℃，反应时间为18 h，优化条件下，收率达90.5%。产品结构和纯度经核磁共振波谱、质谱和高效液相色谱等仪器表征确定，呋虫胺代谢物UF的纯度>98.0%。该化合物可以作为高纯标准品，用于呋虫胺及其代谢物的残留检测。 |
| 关键词：呋虫胺代谢物UF；合成；表征；标准品 |
| 中图分类号：O626.11 文献标识码：A 文章编号：1009-9212（2022）04-0028-05 |
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| Synthesis of Dinotefuran Metabolite UF |
| GUO Hui, CHEN Wu-lian
(Anpel Laboratory Technologies (Shanghai) Inc., Shanghai 201600, China) |
| Abstract：A novel synthetic method of dinotefuran metabolite UF was investigated. The dinotefuran metabolite UF was synthesized from N-methyl-1-imidazolamide and 3-aminomethyltetrahydrofuran using organic base as catalyst. The influencing factors of reaction were investigated and the optimal reaction conditions were determined. Experimental results indicated the optimal condition as followings: the molar ratio of N-methyl-1-imidazolamide to 3-aminomethyltetrahydrofuran was 1.0∶1.0; the catalyst was triethylamine or pyridine, and the molar ratio of catalyst to N-methyl-1-imidazolamide was 1.1∶1.0; the reaction temperature was room temperature; the reaction time was 18 h. Under the above conditions, a yield of the dinotefuran metabolite UF was up to 90.5%. The structure and chemical purity of UF were identified by NMR, MS and HPLC. The chemical purity of dinotefuran metabolite UF was higher than 98.0%. The results showed that the dinotefuran metabolite UF could be used as high purity standard in the determination of dinotefuran and metabolite residue. |
| Key words：dinotefuran metabolite UF; synthesis; characterization; standards |
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作者简介：郭 会（1989—），男，安徽潜山人，工程师，硕士，研究方向：有机标准品的合成（E-mail：guohui@anpel.com.cn）。
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收稿日期：2022-04-11
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