N-甲基氧化吗啉的合成

通过两步反应合成了N-甲基氧化吗啉。第一步,以甲醛、甲酸和吗啉为原料合成了N-甲基吗啉,考察了影响反应的主要因素,得到了较佳工艺条件:n(甲醛)∶n(甲酸)∶n(吗啉)=1.3∶1.2∶1.0,反应温度85~90℃,反应时间4~5 h,在此条件下得到的N-甲基吗啉通过红外光谱验证结构正确,其收率大于90%,产品质量分数大于98%。第二步,以过氧化氢氧化N-甲基吗啉得到N-甲基氧化吗啉,考察了影响反应的主要因素,得到了较佳反应条件:n(过氧化氢)∶n(N-甲基吗啉)=1.4∶1.0,反应温度65~75℃,反应时间6.0 h,得到的N-甲基氧化吗啉结构正确,其收率大于92%,产品质量分数大于99%。

Synthesis of N-Methylmorpholine-N-oxide

N-Methylmorpholine-N-oxide was synthesized by a two-step method.N-Methylmorpholine was synthesized using formaldehyde,formic acid and morpholine in the first step reaction.The main controlling factors in this reaction were investigated and the optimal settings were obtained as follows,n(formaldehyde)∶n(formic acid)∶n(morpholine)=1.3∶1.2∶1.0,reaction temperature as 85~90 ℃,and reaction time as 4~5 h.The structure of the product was characterized by FT-IR.The yield is higher than 90% and purity greater than 98%.In the second step reaction,N-methylmorpholine-N-oxide was obtained by the oxidation of N-methylmorpholine using hydrogen peroxide as the oxidant.The optimal controlling settings were obtained as follows,n(hydrogen peroxide)∶n(N-methylmorpholine)=1.4∶1.0,reaction temperature 65~75 ℃,and reaction time 6.0 h.The yield of N-methylmorpholine-N-oxide is higher than 92% and the purity greater than 99%.