一种2-(2,2-二氟乙氧基)-6-三氟甲基苯磺酰氯的制备方法

Method for preparation of 2-(2,2-difluoroethoxy)-6-(trifluoromethyl)benzene-1-sulfonyl chloride

Abstract

本发明属于有机合成领域,公开了一种制备农用除草剂五氟磺草胺中间体的新路线及新方法,具体涉及一种2?(2,2?二氟乙氧基)?6?三氟甲基苯磺酰氯的制备方法。将2?氯?1?硝基?3?(三氟甲基)?苯甲酸在溶剂的存在下,碳酸钾作为缚酸剂,硫醚化试剂正丙硫醇的作用下15?80℃,反应时间1?8小时;将上述获得物质在溶剂的存在下与四丁基氟化铵,于75?120℃,反应1?6小时;将上述获得的1?氟?2?丙硫基?3?三氟甲基苯在溶剂的存在下与2,2?二氟乙醇和氢化钠在15?70℃,反应1?15小时;上述获得1?(2,2?二氟乙氧基)?2?丙硫基?3?三氟甲基苯与氯气在15?60℃,反应1?6小时。本发明工艺简单、反应温和、产品含量和收率都较高。
The invention belongs to the field of organic synthesis, and discloses a new route and new method for preparation of an agricultural herbicide penoxsulam intermediate, and in particular, relates to a method for preparation of 2-(2,2-difluoroethoxy)-6-(trifluoromethyl)benzene-1-sulfonyl chloride. The method comprises the steps: in the presence of a solvent, with potassium carbonate as an acid binding agent, under the action of a thiolation reagent n-propylmercapatan, and at the temperature of 15-80 DEG C, carrying out a reaction of 2-chloro-1-nitro-3-(trifluoromethyl)-benzoic acid with the reaction time of 1-8 hours; in the presence of the solvent, carrying out a reaction of the obtained substance with tetrabutylammonium fluoride for 1-6 hours at the temperature of 75-120 DEG C; in the presence of the solvent, carrying out a reaction of the obtained 1-fluoro-2-propylthio-3-trifluoromethyl benzene with 2,2-difluoroethanol and sodium hydride for 1-15 hours at the temperature of 15-70 DEG C; and carrying out a reaction of the obtained 1-(2,2-difluoroethoxy)-2-propylthio-3-trifluoromethyl benzene with chlorine gas for 1-6 hours at the temperature of 15-60 DEG C. The method has the advantages of simple process, mild reaction, and relatively high product content and yield.

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Patent Citations (2)

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