以间三氟甲基苯胺(Ⅰ)作为原料,通过与氯甲酸-2-氯乙酯进行选择性的单酰胺化反应(Ⅱ)后,再在氢氧化钠水溶液中经水解重排反应,合成了间三氟甲基-N-羟乙基苯胺(Ⅲ),产物结构经1 H NMR,MS和IR表征.考察了反应溶剂、NaOH用量、反应温度和...以间三氟甲基苯胺(Ⅰ)作为原料,通过与氯甲酸-2-氯乙酯进行选择性的单酰胺化反应(Ⅱ)后,再在氢氧化钠水溶液中经水解重排反应,合成了间三氟甲基-N-羟乙基苯胺(Ⅲ),产物结构经1 H NMR,MS和IR表征.考察了反应溶剂、NaOH用量、反应温度和反应时间对产物收率的影响,实验结果得到:酰胺化反应以二氧六环为溶剂,反应时间3h,反应温度70℃;第二步(Ⅱ)水解重排反应的适宜反应条件为n(间三氟甲基苯胺)∶n(NaOH)=1∶6,反应温度为70℃,反应时间为5h,Ⅲ的总收率可达61%.展开更多
A chemical analytical method for quantitative determination in hydroxyethyl group of hydroxyethyl β cyclodextrin is proposed. The method consists of reacting hydroxyethyl β cyclodextrin with HI in the presence of ca...A chemical analytical method for quantitative determination in hydroxyethyl group of hydroxyethyl β cyclodextrin is proposed. The method consists of reacting hydroxyethyl β cyclodextrin with HI in the presence of catalyst on heating to form the corresponding amounts of ethene and iodoethane. Then react these compounds with bromine to give I 2, which can be easily determined by standard hyposulphite solution. The formulas for calculation of the average substitution degree from titration results are described. The results obtained by this method appeared to be more accurate than those based on 1H NMR method.展开更多
文摘以间三氟甲基苯胺(Ⅰ)作为原料,通过与氯甲酸-2-氯乙酯进行选择性的单酰胺化反应(Ⅱ)后,再在氢氧化钠水溶液中经水解重排反应,合成了间三氟甲基-N-羟乙基苯胺(Ⅲ),产物结构经1 H NMR,MS和IR表征.考察了反应溶剂、NaOH用量、反应温度和反应时间对产物收率的影响,实验结果得到:酰胺化反应以二氧六环为溶剂,反应时间3h,反应温度70℃;第二步(Ⅱ)水解重排反应的适宜反应条件为n(间三氟甲基苯胺)∶n(NaOH)=1∶6,反应温度为70℃,反应时间为5h,Ⅲ的总收率可达61%.
文摘A chemical analytical method for quantitative determination in hydroxyethyl group of hydroxyethyl β cyclodextrin is proposed. The method consists of reacting hydroxyethyl β cyclodextrin with HI in the presence of catalyst on heating to form the corresponding amounts of ethene and iodoethane. Then react these compounds with bromine to give I 2, which can be easily determined by standard hyposulphite solution. The formulas for calculation of the average substitution degree from titration results are described. The results obtained by this method appeared to be more accurate than those based on 1H NMR method.
