对三氟甲氧基-N-羟乙基苯胺的合成

Synthesis of p-(trifluoromethoxy)-N- ethoxyl-benzenaime

摘要:

摘要：由对三氟甲氧基苯胺（1）为原料通过与氯甲酸-2-氯乙酯进行酰胺化反应后，在氢氧化钠水溶液中水解重排，选择性地合成了单-N-羟乙基化反应产物对三氟甲氧基-N-羟乙基苯胺（3），产物结构经1HNMR，13C NMR，MS和IR表征。考察各因素对产物收率的影响，得到最佳反应条件为：酰胺化反应溶剂为二氧六环，反应温度50℃，n(NaOH)︰ n(酰胺化物)=5:1，反应时间7h，3的总收率可达93.7%。 关键词：对三氟甲氧基-N-羟乙基苯胺；对三氟甲氧基苯胺；氯甲酸-2-氯乙酯；合成 中图分类号：O625.63 基金项目：国家自然科学基金资助项目(20905057)

Abstract:

Abstract：P-(trifluoromethoxy)-N-hydroxyethyl-benzenamine (3) was selectively synthesised using p-(trifluoromethoxy)-benzenamine (1) as the raw material . The product was obtained by the route during amidation with chloroethyl chloroformate，then hydrolyzed and rearrangement in NaOH aqueous solution，the structure of products were confirmed by 1H NMR，13C NMR，Ms and IR．Factors on yield of products were studied，it was found that the yield of 3 can reach 93.7% under the optimal reaction condition of n(NaOH)：n(amide) with 5:1 at 50℃ for 7h in dioxane ． Keywords：p-(trifluoromethoxy)-N- hydroxyethyl-benzenamine；p-(trifluoromethoxy)-benzenamine；chloroethyl chloroformate；synthesis Foundation item：Natural Science Foundation of China(20905057)