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
基金项目:
作者单位E-mail
万灵子 上海工程技术大学 化学化工学院  
卜乐号 上海工程技术大学 化学化工学院  
刘耀威 上海工程技术大学 化学化工学院  
茆勇军 上海工程技术大学 化学化工学院 yongjun.mao@hotmail.com 
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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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