| 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
4-氯-2-氰基-5-（4-甲基苯基）咪唑的合成工藝優(yōu)化 |
| 王 濤
（上海生農生化制品股份有限公司，上海 201108） |
| 摘 要：以2，2-二氯-4'-甲基苯基乙酮為主要原料，與羥胺鹽先形成單肟化物，一鍋法與40%乙二醛水溶液進(jìn)行關(guān)環(huán)反應，得到1-羥基-4-（4'-甲基苯基）-2-甲肟基咪唑-3-氧化物，然后該氧化物先在氯化亞砜的參與下，進(jìn)行脫水反應得到氰基化物，一鍋法再在二氯化硫的參與下進(jìn)行氯化反應得到4-氯-2-氰基-5-（4'-甲基苯基）咪唑。研究了物料配比、反應溫度、反應時(shí)間等影響因素，優(yōu)化后4-氯-2-氰基-5-（4'-甲基苯基）咪唑的總收率達80.5%。該合成方法原料廉價(jià)易得，收率高，反應過(guò)程簡(jiǎn)單。 |
| 關(guān)鍵詞：氰霜唑；4-氯-2-氰基-5-（4'-甲基苯基）咪唑；合成 |
| 中圖分類(lèi)號：TQ460.6 文獻標識碼：A 文章編號：1009-9212（2020）06-0032-05 |
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| Synthesis of 4-Chloro-2-cyano-5- (4'-methylphenyl)-imidazole |
| WANG Tao
(Shanghai Shengnong Pesticide Co., Ltd., Shanghai 201108, China) |
| Abstract：1-Hydroxy-4-(4'-methylphenyl)-2-oxyiminomethylimidazole-3-oxide was synthesized using 2,2-dichloro-4'-methyl acetophenone as the starting material followed a series reactions including oxime formation with hydroxylamine salt and cyclization with 40% aqueous solution of glyoxal. And the 4-Chloro-2-cyano-5-(4'-methylphenyl)-imidazole was obtained using the Oxide through reactions including dehydration with thionyl chloride and then chlorination with sulfur dichloride. The effect of material ratio, reaction temperature and reaction time was discussed, and the total yield was 80.5% under the optimized condition. This new synthetic method had the advantages including commercialized raw materials, high yield and simple process. |
| Key words：cyazofamid; 4-chloro-2-cyano-5-(4'-methylphenyl)-imidazole; synthesis |
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作者簡(jiǎn)介：王 濤（1982—），男，湖北宜昌人，工程師，博士，主要從事藥物合成及工藝研究（E-mail：noblerwang@163.com）。
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收稿日期：2020-10-30
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