| 第 52 卷第 4 期 |  | Vol. 52 No. 4 | | 2022 年 8 月 | Aug 2022 |
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所屬欄目：農藥及中間體
呋蟲(chóng)胺代謝物UF的合成研究 |
| 郭 會(huì )，陳武煉
（上海安譜實(shí)驗科技股份有限公司，上海 201600） |
| 摘 要：研究了一種全新的呋蟲(chóng)胺代謝物UF的合成方法，即以N-甲基-1-咪唑甲酰胺和3-氨基甲基四氫呋喃為原料，在有機堿催化下室溫反應得到呋蟲(chóng)胺代謝物UF�？疾炝朔磻挠绊懸蛩�，確定了優(yōu)化反應條件：n（N-甲基-1-咪唑甲酰胺）∶n（3-氨基甲基四氫呋喃）=1.0∶1.0，催化劑使用三乙胺或吡啶，n（催化劑）∶n（N-甲基-1-咪唑甲酰胺）=1.1∶1.0，反應溫度為25 ℃，反應時(shí)間為18 h，優(yōu)化條件下，收率達90.5%。產(chǎn)品結構和純度經(jīng)核磁共振波譜、質(zhì)譜和高效液相色譜等儀器表征確定，呋蟲(chóng)胺代謝物UF的純度>98.0%。該化合物可以作為高純標準品，用于呋蟲(chóng)胺及其代謝物的殘留檢測。 |
| 關(guān)鍵詞：呋蟲(chóng)胺代謝物UF；合成；表征；標準品 |
| 中圖分類(lèi)號：O626.11 文獻標識碼：A 文章編號：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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作者簡(jiǎn)介：郭 會(huì )（1989—），男，安徽潛山人，工程師，碩士，研究方向：有機標準品的合成（E-mail：guohui@anpel.com.cn）。
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收稿日期：2022-04-11
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