摘要
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4～5h，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6．0h，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％。
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%.
出处
《青岛科技大学学报（自然科学版）》
CAS
2008年第4期283-286,共4页
Journal of Qingdao University of Science and Technology:Natural Science Edition
