CAJ | 학술논문

以4个不同结构的芳胺为原料，经过N-烷基化，N-氯乙酰化，酯化，酯交换反应合成了4个2-羟基乙酰胺类化合物,它们都是重要的农药中间体。其中N-(4-三氟甲基苯基)-N-异丙基-2-羟基乙酰胺的合成：控制温度在10～20 ℃,向4-三氟甲基苯胺，冰醋酸与丙酮的混合液中慢慢加入硼氢化钾，加完后20 ℃反应2 h得到产品N-异丙基-4-三氟甲基苯胺，产率86.0%。升温至40 ℃，向N-异丙基-4-三氟甲基苯胺、甲苯混合液中滴加氯乙酰氯,滴完后升温至75 ℃,通氮气反应2 h得到产品N-(4-三氟甲基苯基)-N-异丙基-2-氯乙酰胺,产率92.9%。 N-(4-三氟甲基苯基)-N-异丙基-2-氯乙酰胺,甲醇,醋酸钾,三乙胺,碳酸钾,回流反应17 h,得到产品N-(4-三氟甲基苯基)-N-异丙基-2-羟基乙酰胺，产率88.2%，总收率为70.5%。产品结构经质谱和核磁确定。
이4개불동결구적방알위원료，경과N-완기화，N-록을선화，지화，지교환반응합성료4개2-간기을선알류화합물,타문도시중요적농약중간체。기중N-(4-삼불갑기분기)-N-이병기-2-간기을선알적합성：공제온도재10～20 ℃,향4-삼불갑기분알，빙작산여병동적혼합액중만만가입붕경화갑，가완후20 ℃반응2 h득도산품N-이병기-4-삼불갑기분알，산솔86.0%。승온지40 ℃，향N-이병기-4-삼불갑기분알、갑분혼합액중적가록을선록,적완후승온지75 ℃,통담기반응2 h득도산품N-(4-삼불갑기분기)-N-이병기-2-록을선알,산솔92.9%。 N-(4-삼불갑기분기)-N-이병기-2-록을선알,갑순,작산갑,삼을알,탄산갑,회류반응17 h,득도산품N-(4-삼불갑기분기)-N-이병기-2-간기을선알，산솔88.2%，총수솔위70.5%。산품결구경질보화핵자학정。
N-Aryl-N-isopropyl-2-hydroxyacetamides are a series of important intermediates of useful pesticides.Four N-aryl-N-isopropyl-2-hydroxyacetamides were prepared from four arylamines with different structure through N-alkylation,N-chloroacetylation,esterification and transesterification.Thus,keeping temperature at 10-20 ℃,potassium borohydride was added in parts to the solution of 4-trifluoromethylaniline and acetone in glacial acetic acid.It was then stirred at 20 ℃ for two hours to get N-isopropyl-4-trifluoromethylaniline,in 86% yield.Chloroacetyl chloride was added dropwise at 40 ℃ to the solution of N-isopropyl-4-trifluoromethylaniline in toluene and the temperature was raised to 75 ℃.The reaction lasted for two hours at this temperature with nitrogen bubbling through the solution.N-(4-Trifluoromethylphenyl)-N-isopropyl-2-choloroacetamide was obtained in 92.9% yield.N-(4-Trifluoromethylphenyl)-N-isopropyl-2-hydroxyacetamide was obtained by refluxing the mixture of N-(4-trifluoromethylphenyl)-N-isopropyl-2-chroloroacetamide,methanol,triethylamide,potassium acetate and potassium carbonate in 88.2% yield.The overall yield was 70.5%.The product was identified by 1 HNMR and CIMS.