| 第 50 卷第 4 期 |  | Vol. 50 No. 4 | | 2020 年 8 月 | Aug 2020 |
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所屬欄目：農藥及中間體
殺線(xiàn)蟲(chóng)劑Tioxazafen關(guān)鍵中間體2-噻吩甲酸的制備研究 |
| 張廣平1，王梓鑒2
（1. 湖南海利常德農藥化工有限公司，湖南 常德 415001；2. 長(cháng)沙嘉橋生物科技有限公司，湖南 長(cháng)沙 410000） |
| 摘 要：2-噻吩甲酸（T2）是殺線(xiàn)蟲(chóng)劑Tioxazafen的關(guān)鍵中間體。以噻吩和乙酰氯為原料制備2-噻吩乙酮（T1），隨后用次氯酸鈉氧化得到產(chǎn)品2-噻吩甲酸（T2）。T1的優(yōu)化制備條件為：n（噻吩）∶n（乙酰氯）∶n（三氯化鋁）=1.00∶1.15∶1.15，反應溫度為25 ℃，噻吩滴加到乙酰氯和三氯化鋁的二氯乙烷溶液中；T2的優(yōu)化制備條件為：n（T1）∶n（次氯酸鈉）=1.00∶3.15，氧化溫度為30 ℃。2步反應總收率87.84%，純度98.23%（HPLC）。 |
| 關(guān)鍵詞：Tioxazafen；2-噻吩乙酮；2-噻吩甲酸 |
| 中圖分類(lèi)號：TQ251.2 文獻標識碼：A 文章編號：1009-9212（2020）04-0018-03 |
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| Preparation of the Key Intermediate of the Nematicide Tioxazafen: 2-Thiophenecarboxylic Acid |
| ZHANG Guang-ping1,WANG Zi-jian2
(1. Hunan Haili Changde Pesticide Chemical Co.,Ltd.,Changde 415001, China; 2. Chang Sha Jia Qiao Biotech Co.,Ltd.,Changsha 410000, China) |
| Abstract：2-Thiophenecarboxylic acid (T2) is a key intermediate of the nematicideTioxazafen. 2-Thiophene ethyl ketone (T1) was prepared fromthiophene and acetyl chloride. And then T1 was oxidized using sodium hypochlorite to give the product T2. The optimized preparation conditions of T1 were as followings: a molar ratiobewteenthiophene, acetyl chloride and aluminum trichloride was of 1.00∶1.15∶1.15; the reaction temperature was of 25 ℃; thiophene was added dropwise to a solution of acetyl chloride and aluminum trichloride in dichloroethane. The optimized preparation conditions of T2 were as followings: the oxidation temperature was of 30 ℃; and n(T1)∶n(sodium hypochlorite) was of 1.00∶3.15. The total yield of the two-step reactions was 87.84% with a purity of 98.23% (HPLC). |
| Key words：Tioxazafen; 2-acetylthiophene; 2-thiophenecarboxylic acid |
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基金項目：國家自然科學(xué)基金項目（21672057）。
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作者簡(jiǎn)介：張廣平（1964—），男，湖南澧縣人，工程師，主要從事農藥精細化工產(chǎn)品開(kāi)發(fā)及工程化工作（E-mail：223208906@qq.com）。
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收稿日期：2020-07-27
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