| 第 50 卷第 6 期 |  | Vol. 50 No. 6 | | 2020 年 12 月 | Dec 2020 |
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所屬欄目：農藥及中間體
1-甲基-3-（二氟甲基）-1H-吡唑-4-羧酸的綠色合成 |
| 尚 宇，黃 艷，張 淳，郭亞飛，李 飛
（陜西省環(huán)境監測中心站，陜西 西安 710054） |
| 摘 要：以二氟乙酸乙酯為原料，經(jīng)Claisen酯縮合、乙氧亞甲基化、環(huán)化、水解反應合成了1-甲基-3-（二氟甲基）-1H-吡唑-4-羧酸，并優(yōu)化了反應條件。優(yōu)化反應條件下，總收率≥44%，純度≥99%。中間體及產(chǎn)物結構經(jīng)1H NMR、MS確認。該工藝操作簡(jiǎn)單，條件溫和。 |
| 關(guān)鍵詞：1-甲基-3-（二氟甲基）-1H-吡唑-4-羧酸；二氟乙酸乙酯；合成 |
| 中圖分類(lèi)號：S482.2 文獻標識碼：A 文章編號：1009-9212（2020）06-0025-04 |
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| A Green Route for the Synthesis of 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic Acid |
| SHANG Yu, HUANG Yan, ZHANG Chun, GUO Ya-fei, LI Fei
(Shaanxi Environmental Monitoring Center, Xi′an 710054, China) |
| Abstract：3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid was prepared using ethyl difluoroacetate as starting material through a series of reactions including ester condensation reaction, ethoxylation, cyclization, and hydrolysis reaction. Its structure was conformed by 1H NMR and MS. Under the optimal reaction conditions, the total yield was over 44% based on the amount of ethyl difluoroacetate used while the purity was up to 99%. This process is simple, warm and economical. |
| Key words：3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid; ethyl difluoroacetate; synthesis |
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作者簡(jiǎn)介：尚 宇（1983—），男，遼寧撫順人，工程師，主要從事環(huán)境監測工作（E-mail：523588666@qq.com）。
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收稿日期：2020-11-23
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