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[目的]2-氧代环己烷基磺酸盐是合成N-(2-三氟甲基-4-氯苯基)-2-氧代环己烷基磺酰胺(L-13)的重要中间体,为了进一步提高其收率和纯度,研究了2-氧代环己烷基磺酸盐合成的反应条件。同时研究了用五氧化二磷与硫酸反应制备三氧化硫的条件。[结果]合成2-氧代环己烷基磺酸盐的最佳投料摩尔比是三氧化硫∶二氧六环∶环己酮为1∶1.1∶1.1,最佳反应温度-15~-20℃,最佳反应时间为4 h,溶剂的用量是三氧化硫∶二氯乙烷为1 g∶5.06 mL。在后处理过程中用氢氧化钙除掉硫酸,经碱中和生成的磺酸钾盐的质量要好于磺酸钠盐。[结论]投料比、反应温度、溶剂用量和后处理方法对2-氧代环己烷基磺酸盐的收率和品质影响很大,磺酸钾盐的收率可达71.2%,其能够满足L-13的合成要求。
[Objective] The 2-oxocyclohexane sulfonate is important for the synthesis of N- (2-trifluoromethyl-4-chlorophenyl) -2-oxocyclohexylsulfonamide (L-13) In order to further improve its yield and purity, the reaction conditions of 2-oxocyclohexylsulfonate synthesis were studied. The conditions for the production of sulfur trioxide from phosphorus pentoxide and sulfuric acid were also studied. [Result] The optimal molar ratio of 2-oxocyclohexane sulfonate was 1: 1.1: 1.1 of sulfur trioxide: dioxane: cyclohexanone. The optimum reaction temperature was -15 ~ -20 ℃, the best reaction time is 4 h, the amount of solvent is sulfur trioxide: dichloroethane is 1 g: 5.06 mL. In the post-treatment process with calcium hydroxide to remove sulfuric acid, the quality of the sulfonic acid potassium salt generated by alkali and sodium sulfonate is better than the salt. [Conclusion] The yield and quality of 2 - oxocyclohexane sulfonate were greatly influenced by the feed ratio, reaction temperature, the amount of solvent and the post - treatment method. The yield of sulfonate potassium salt was 71.2% Meet the synthetic requirements of L-13.