| 苯嘧磺草胺的新合成方法 |
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| 引用本文： | 万灵子,卜乐号,刘耀威,茆勇军. 苯嘧磺草胺的新合成方法[J]. 化学通报, 2019, 82(9): 826-830 |
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| 作者姓名： | 万灵子 卜乐号 刘耀威 茆勇军 |
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| 作者单位： | 上海工程技术大学化学化工学院 上海201620;上海工程技术大学化学化工学院 上海201620;上海工程技术大学化学化工学院 上海201620;上海工程技术大学化学化工学院 上海201620 |
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| 摘 要： | 设计并完成苯嘧磺草胺及其关键中间体的合成工艺路线，使其具备工业化生产潜力。采用氯磺酰异氰酸酯、叔丁醇、N-甲基-N-异丙基胺等作为起始原料，制备了关键中间体N-甲基-N-异丙基氨基磺酰胺，3步反应总收率~75%；采用2-氯-4-氟苯甲酸为原料，经过硝化、酰氯化、缩合、催化氢化还原、氨酯交换、甲基化反应制备了苯嘧磺草胺。共计8步反应制备得到苯嘧磺草胺，总收率为48.6%，纯度98.6%，产物与中间体经NMR、MS等进行了表征。
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| 关 键 词： | 除草剂 苯嘧磺草胺 N-甲基-N-异丙基氨基磺酰胺 合成工艺 |
| 收稿时间： | 2019-05-11 |
| 修稿时间： | 2019-06-13 |
New Synthesis of Saflufenacil |
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| WAN Lingzi,BU Lehao,LIU Yaowei and Mao Yongjun. New Synthesis of Saflufenacil[J]. Chemistry, 2019, 82(9): 826-830 |
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| Authors: | WAN Lingzi BU Lehao LIU Yaowei Mao Yongjun |
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| Affiliation: | College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science |
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| Abstract: | The synthetic process of saflufenacil and its key intermediates is designed and completed, which has the potential for industrial manufacturing. Chlorosulfonyl isocyanate, t-butanol and N-methyl-N-isopropylamine are adopted as the starting materials, the key intermediate N-methyl-N-isopropylaminosulfonamide is prepared in 75% yield over 3 steps. Saflufenacil is prepared from 2-chloro-4-fluorobenzoic acid through nitration, chloridization, condensation, catalytic hydrogenation reduction, aminolysis and methylation reactions. Saflufenacil is obtained in 48.6% yield over 8 steps and 98.6% purity. The final products and the intermediates are characterized by NMR and MS. |
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| Keywords: | Herbicide Saflufenacil N-methyl-N-isopropylaminosulfonamide Synthesis process |
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