| 第 49 卷第 3 期 |  | Vol. 49 No. 3 | | 2019 年 6 月 | Jun 2019 |
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所屬欄目：農藥及中間體
提高1氫-1，2，4-三氮唑收率及品質(zhì)的研究 |
| 朱 鵬，徐剛亮，劉志勇*
（江蘇劍牌農化股份有限公司，江蘇 建湖 224700） |
| 摘 要：以甲酰胺與水合肼為原料，采用液面下滴加水合肼、引入乙二醇作為反應溶劑、應用結晶-過(guò)濾-漂洗-烘干的后處理方式，合成了1氫-1，2，4-三氮唑，并對其合成工藝條件進(jìn)行了研究。優(yōu)化的反應條件為：m（乙二醇）＝50% m（水合肼），n（甲酰胺）∶n（水合肼）＝2.1∶1.0，反應溫度為168℃，反應時(shí)間為120 min。優(yōu)化條件下，三氮唑收率為86.8%（以甲酰胺計三氮唑）或91.1%（以水合肼計），產(chǎn)品含量為98%，m.p.120~121℃。副產(chǎn)氨水中甲酰胺的含量為0.2%，水合肼的含量為0.1%。 |
| 關(guān)鍵詞：三氮唑；甲酰胺；水合肼；乙二醇 |
| 中圖分類(lèi)號：TQ21 文獻標識碼：A 文章編號：1009-9212（2019）03-0007-05 |
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| Improvement of Yield and Quality of 1H-1,2,4-Triazole |
| ZHU Peng, XU Gang-liang, LIU Zhi-yong*
(Jiangsu Sword Agrochemicals Co., Ltd., Jianhu 224700, China) |
| Abstract：1H-1,2,4-Triazole was synthesized as follows: formamide and hydrazine hydrate were used as raw materials, the hydrazine hydrate was added under the liquid surface, ethylene glycol was used as the reaction solvent, and crystallization-filtration-rinsing-drying was applied as the post-processing method. The parameters of the reaction were optimized. Optimal conditions were as followings: m(ethylene glycol) = 50% m(hydrazine hydrate), n(formamide)∶n(hydrazine hydrate)=2.1:1.0, reaction temperature of 168℃, reaction time of 120 min. The experimental results showed that the yield of triazole calculated based on the amount of formamide was up to 86.8%, the yield of triazole calculated based on the amount of hydrazine hydrate was up to 91.1%, the purity of product was of 98% with a melting point range of 120 to121℃. The concentrations of formamide and hydrazine hydrate were 0.2% and 0.1% in the by-product ammonia water, respectively. |
| Key words：triazole; formamide; hydrazine hydrate; ethylene glycol |
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作者簡(jiǎn)介：朱 鵬（1989-），男，江蘇濱海人，碩士研究生，研究方向：農藥合成及工藝研究（E-mail：zhupeng@swordchem.com）。
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聯(lián) 系 人：劉志勇，高級工程師，研究方向：農藥合成及工藝研究（E-mail：liuzhiyong@swordchem.com）。
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收稿日期：2019-05-29
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