| 万灵子,卜乐号,刘耀威,茆勇军.化学通报,2019,82(9):826-830. |
| 苯嘧磺草胺的合成 |
| New Synthesis of Saflufenacil |
| 投稿时间：2019-05-11 修订日期：2019-06-13 |
| DOI： |
| 中文关键词: 除草剂 苯嘧磺草胺 N-甲基-N-异丙基氨基磺酰胺 合成工艺 |
| 英文关键词:Herbicide, Saflufenacil, N-methyl-N-isopropylaminosulfonamide, Synthesis process |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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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