【摘要】 探索以邻硝基苯酚、1-氯丙酮为原料,铂碳为催化剂,通过O-烷基化、还原、环合反应,合成3-甲基-3,4-二氢-2H-1,4-苯并噁嗪。利用四因素三水平正交实验设计研究了还原-环合反应过程中溶剂效应、反应温度、搅拌时间、反应压力对标题化合物产率的影响,确定了合成标题化合物的优化工艺条件为:以甲苯为溶剂,反应温度45~50℃,反应时间15 h,反应压力2.0 MPa,合成收率达92.5%。产物结构经红外光谱、核磁共振和元素分析进行了表征。本方法原料廉价易得,产物收率高,适用于工业化生产。更多还原

【Abstract】 A 3-methyl-3,4-dihydro-2H-1,4-benzoxazine synthetic route was investigates which consists of O-alkylation, reduction, and ring closure reactions, and o-nitrophenol and 1-chloro-acetone were used as the reactants and with Pt/C as the catalyst. Factors affecting reaction yield such as solvent, reaction temperature, stirring time and reaction pressure were studied under orthogonal experimental design. The optimum synthetic conditions were found as: using toluene as the solvent under reaction temperature of 45~50℃, stirring time of 15 h and pressure of 2.0 MPa, the yield could reach to 92.5%. Moreover, the structures of the obtained compounds were characterized by IR, 1H-NMR, 13C-NMR and elemental analysis. This study shows that the proposed synthetic route is simple with high yields, and the raw materials are cheap and easy to obtain.更多还原