1-甲基-2-硝基亚胺基-5-甲基-六氢化-1,3,5-三嗪的合成

Synthesis of 1-methyl-2-nitroimino-5-methyl-1,3,5-triazacyclohexane

在无溶剂、微波辐射下,以N-甲基硝基胍、甲胺水溶液及甲醛为原料合成1-甲基-2-硝基亚胺基-5-甲基-六氢化-1,3,5-三嗪。对产物进行红外光谱、核磁共振分析和熔点测定。用均匀设计方法安排实验,对反应温度、反应时间及反应物用量等影响因素进行考察,回归方程进行优化,经实验验证得反应的最佳条件:反应温度55℃,反应时间50s,N-甲基硝基胍、甲醛、甲胺的摩尔比为1∶2.3∶2,收率达69.7%。

1-methyl-2-nitroimino-5-methyl-1,3,5-triazacyclohexane is synthesized from methyl nitroguanidine, formaldehyde and methylamine with microwave irradiation and no solvent. Structures of products were identified by means of micro-melting point measuring instrument, IR and ^1H NMR spectra. By uniform experiment design, effects of reaction temperature, irradiation time and reactants ratio etc. on reaction were studied, Optimal reaction conditions were determined as follows： reaction temperature 55℃, the irradiation time 50s,the ratio n（methyl nitroguanidine） ： n（formaldehyde） ： n（methylamine） =1：2.3：2.Yield of products can reach 69.7%.