机构地区: 青岛科技大学化工学院
出 处: 《化工科技》 2016年第1期37-40,共4页
摘 要: 研究了对甲苯磺酰甲基甲酰胺脱水合成对甲苯磺酰甲基异腈,考察了溶剂种类和用量、原料配比、反应时间等因素对反应结果的影响,得到了最佳反应条件,即m(对甲苯磺酰甲基甲酰胺)=6g,V(二氯甲烷)=30mL,n(酰胺)∶n(三乙胺)∶n(三氯氧磷)=1∶5∶1.1,反应温度为-5℃,滴加时间为20min,反应时间为60min,沉降时间为60min。在上述条件下,对甲苯磺酰甲基异腈的收率和纯度分别为83.3%和98.0%。其结构经FT-IR和NMR分析确证。 Tosylmethyl isocyanide was prepared by using N-(p-tolysulfonylmethyl)-formamide as the starting material.The effects of factors,such as kind and dosage of solvent,amount of raw materials,and reaction time,were examined.The optimum conditions were obtained as follows:N-(p-tolysulfonylmethyl)-formamide 6g,n(amide)∶n(triethylamine)∶ n(phosphorus oxychloride)=1∶5∶1.1,solvent dichloromethane 30 mL,reaction temperature-5 ℃,and reaction time 60 min.Under the above reaction conditions,the yield and purity of tosylmethyl isocyanide were more than 83.3% and98.5%,respectively.Its structure was also confirmed by FT-IR and NMR.
关 键 词: 对甲苯磺酰甲基甲酰胺 对甲苯磺酰甲基异腈 合成
领 域: [化学工程]