摘要
提供了一种微波法制备N-((4-氨基-2-甲基嘧啶-5-基)甲基)甲酰胺的新方法。在一定条件下,使用液体甲醇钠与盐酸乙脒进行游离反应,滤除氯化钠,蒸除甲醇得游离的乙脒,再与定量的N-(3-(2-氯苯基)-2氰基烯丙基)-甲酰胺和甲醇于微波中进行环合反应得目标产物并进行了数据表征。该工艺的最佳实验条件为0.13 moL盐酸乙脒与0.085 moL N-(3-(2-氯苯基)-2氰基烯丙基)-甲酰胺和10 mL甲醇在50℃条件下于微波中反应4.5 min得N-((4-氨基-2-甲基嘧啶-5-基)甲基)甲酰胺13.9 g,含量93.0%,收率90.4%。本方法具有反应时间短,收率高,易操作等特点,为工业化奠定了一定基础。
A new microwave method for the preparation of N-（（4-amino-2-methylpyrimidin-5-yl）methyl）-formamide was introduced. Under certain conditions, the free reaction between liquid sodium methoxide and acetamidine hydrochloride was carried out. The sodium chloride was removed by filtration, and methanol was distilled off to obtain the free acetamidine, then the three compounds（the free acetamidine,quantitative N-（3-（2-chlorophenylamino）-2-cyanoallyl） formamide and methanol） were cyclized in microwave to obtain the desired product. The optimal experimental conditions for this process were determined as follows： acetamidine hydrochloride 0.13 moL, N-（3-（2-chlorophenyl）-2-cyanoallyl）-carboxamide 0.085 moL, methanol 10 mL, cyclizing temperature 50°C,the time in microwave 4.5 min.Under above conditions, 13.9 g product was prepared, its content was 93.0%, the yield was 90.4%. The method has many advantages including short reaction time, high yield and easy operation, and lays a certain foundation for industrialization.
作者
周宏
白跃飞
刘姝宏
吴晓璟
皮昌桥
ZHOU Hong;BAI Yue-fei;LIU Shu-hong;WU Xiao-jing;PI Chang-qiao(Northeast Pharmaceutical Group Co.,Ltd., Liaoning Shenyang 110027, China)
出处
《辽宁化工》
CAS
2018年第5期404-406,409,共4页
Liaoning Chemical Industry
