| 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
3，5-二氯苯異氰酸酯的合成研究 |
| 劉 源1，2，劉建雄3，劉雙瑾3，胡 偉3，杜升華1，2
（1. 湖南化工研究院有限公司 國家農藥創(chuàng )制工程技術(shù)研究中心，湖南 長(cháng)沙 410014；2. 農用化學(xué)品湖南省重點(diǎn)實(shí)驗室，湖南 長(cháng)沙 410014；3. 湖南海利常德農藥化工有限公司，湖南 常德 415000） |
| 摘 要：采用二（三氯甲基）碳酸酯（BTC）代替傳統光氣合成了3，5-二氯苯基異氰酸酯。研究了影響反應收率的因素，優(yōu)化條件為：以甲苯為溶劑，n（BTC）∶n（3，5-二氯苯胺）=1.0∶2.0，滴加溫度0~5 ℃，回流溫度108 ℃，反應時(shí)間3 h。優(yōu)化條件下產(chǎn)物收率95.5%，純度99.4%。產(chǎn)物結構經(jīng)紅外光譜、核磁共振儀、氣質(zhì)聯(lián)用儀確證。與光氣法相比，BTC法具有操作簡(jiǎn)便、收率高、工藝安全等優(yōu)點(diǎn)。 |
| 關(guān)鍵詞：3，5-二氯苯異氰酸酯；固體光氣；合成 |
| 中圖分類(lèi)號：TQ226.63 文獻標識碼：A 文章編號：1009-9212（2022）04-0025-03 |
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| Synthesis of 3,5-Dichlorophenylisocyanate |
| LIU Yuan1,2, LIU Jian-xiong3, LIU Shuang-jin3, HU Wei3, DU Sheng-hua1,2
(1. Hunan Research Institute of Chemical Industry Co., Ltd., National Engineering Research Centre for Agrochemicals, Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. Hunan Haili Changde Pesticide Chemical Co., Ltd., Changde 415000, China) |
| Abstract：Synthesis of 3,5-dichlorophenylisocyanate was tried using BTC instead of traditional phosgene. The factors affecting the reaction yield were studied, and a yield of 95.5% and a purity of 99.4% were obtained under the following optimized conditions: toluene as solvent, the molar ratio of BTC to 3,5-dichloroaniline of 1.0∶2.0; the dropping temperature of 0~5 ℃, reflux temperature of 108 ℃, reaction time of 3 h. The structure of the product was confirmed by IR, 1H NMR, and GC-MS. Compared with the phosgene method, the BTC method had the advantages of simple operation, high yield, and process safety. |
| Key words：3,5-dichlorophenylisocyanate; BTC; synthesis |
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作者簡(jiǎn)介：劉 源（1988—），男，湖南湘鄉人，助理研究員，碩士，研究方向：農藥工藝開(kāi)發(fā)（E-mail：349942174@qq.com）。
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收稿日期：2022-07-04
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