3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲砜基乙基)-1,2-苯二甲酰胺的合成

Synthesis of 3-iodo-N1-(2-methyl-4-(perfluoropropan-2-yl)-N2-(2-methyl-1-(methylsulfinyl)propan-2-yl)phenyl)phthalamide

摘要:

以邻苯二甲酸酐为原料，经酰胺化、氧化、碘化反应制得3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲硫基乙基)-1,2-苯二甲酰胺。讨论了反应物料摩尔比、催化剂用量、反应温度、反应时间等因素对产品收率的影响。优化后四步反应总收率61.1%，含量96.5%。产物及中间体结构经1HNMR和ESI-MS确证。通过对钯碳的回收套用大大降低了成本。该合成路线具有原料易得，操作简便，收率高等优点，具有较好的工业化应用前景。

Abstract:

3-iodo-N1-(2-methyl-4-(perfluoropropan-2-yl)-N2-(2-methyl-1-(methylsulfinyl)propan-2-yl)phenyl)phthalamide was synthesized from isobenzofuran-1,3-dione via amidation, oxidization, iodination. The effects of materials' mole ratio, the amount of catalyst, reaction temperature and time on the yield of product were studied. In the improved process, after 4 steps, the total yield could reach 61.1%, and the purity of product was 96.5%. Structures of all intermediates and target product were characterized by 1HNMR and ESI-MS. The recovery and reuse of Palladium carbon could reduce the economic costs. This synthetic route is characterized by cost-effectiveness, simple operation and high yield , which are very promising in industrialization.