【摘要】 以甲酸铵为氢源和氮源,N,N-二甲基甲酰胺为溶剂,探讨了甲酸铵直接还原胺化乙酰丙酸制备5-甲基-2-吡咯烷酮的反应途径及机理。通过实验分别考察了反应温度、反应时间、乙酰丙酸与甲酸铵的总质量分数和物质的量比、体系pH值等反应条件对5-甲基-2-吡咯烷酮得率的影响趋势。结果表明,适当提高反应温度、延长反应时间、提高乙酰丙酸与甲酸铵的物质的量比和总质量分数、增加体系pH值均有利于提高5-甲基-2-吡咯烷酮的得率。同时,考察了不同溶剂和乙酰丙酸衍生物在该反应体系中的应用,结果表明极性非质子溶剂甲酰胺、N,N-二甲基乙酰胺、二甲亚砜亦可作为该中体系反应的反应溶剂,乙酰丙酸甲酯、α-当归内酯可作为反应底物在该体系下制备5-甲基-2-吡咯烷酮。更多还原

【Abstract】 The reductive amination of levulinic acid with ammonium formate as hydrogen and nitrogen donor to synthesize 5-methyl-2-pyrrolidone(5-Me P) in DMF solvent was developed and the mechanism of this process was proposed.The effects of various reaction conditions including temperature,reaction time,mass fraction and molar ratio of levulinic acid with ammonium formate and pH value on 5-methyl-2-pyrrolidone yield were investigated.Meanwhile,different solvents and levulinate derivatives were investigated in this system.The results showed that the properly increasing temperature,reaction time,the molar ratio and total mass fraction of levulinic acid and ammonium formate,and the pH value of system could improve the yield of 5-methyl-2-pyrrolidone.The polar aprotic solvents including formamide,DMA,DMSO and levulinate derivatives,such as methyl levulinate and α-angelica lactone,could also be respectively used as solvents and substrates in this system,too.更多还原