臭氧化法制备N-Boc-(甲氨基)乙醛

Preparation of N-Boc-(Methylamino)Acetaldehyde by Ozonization Method

以N-甲基烯丙胺和二碳酸二叔丁酯为原料,在乙醇中缩合得到N-Boc-甲基烯丙胺,再以乙酸乙酯为溶剂经臭氧臭氧化,用NaHSO_(3)还原分解,经萃取、蒸馏,制备N-Boc-(甲氨基)乙醛。采用L16(45)正交实验确定了最优臭氧化温度为5~10℃、反应时间为3 h、臭氧流量为0.04 m^(3)/h,粗产物用乙醚萃取,获得目标产物收率78.7%,纯度99.2%(HPLC),并用IR、^(1)H NMR、^(13)C NMR和MS表征了产物的结构。

N-Methylallylamine and di-tert-butyl dicarbonate were used as raw materials,condensed in ethanol to obtain N-Boc-methylallylamine,then ozonated with ethyl acetate as solvent reduced by NaHSO_(3),and N-Boc-(methylamino)acetaldehyde was prepared by extraction and distillation.The optimum ozonation temperature of 5~10℃,reaction time of 3h,and ozone flow rate of 0.04 m^(3)/h were determined using L16(45)orthogonal experiments,the crude product was extracted with ether to obtain the target product in 78.7%yield and 99.2%purity(HPLC),and the structure of the product was characterized by IR,^(1)H NMR,^(13)C NMR and MS.