Synthsis Of 1-ethyl-2-aminomethyl Pyrrolidine From Tetrahydro-2-methylfuran

1-Ethyl-2-Aminomethyl Pyrrolidine（EAMP）is an important intermediate in the synthesis of several drugs as well as in the industry of pesticides,dyes and coatings.In view of the safety and environmental problems of the existing processes,it is of significance to explore a green process of EAMP.Based on the existing processes of EAMP,a novel route of EAMP was proposed,in which 2-methyltetrahydrofuran was conversed to EAMP through three step,amination,ammoxidation and hydrogenation.（1）The amination of 2-methyltetrahydrofuran on aluminum and ZSM-5 zeolite catalyst was investigated.Two alumina catalysts and seven ZSM-5 molecular sieves with different Si/Al ratios were used in the amination,and the ZSM-5 zeolite catalyst with Si/Al ratio of 46 were screened out.Further,the ZSM-5 with Si/Al ratio of 46 modified by Cu,Ce,K,La and P were tested.The microstructure of aluminum based catalysts and ZSM-5 catalysts was characterized by XRD and BET,it was found that the modification of P changes the pore microstructure of zeolite catalyst,and greatly improves the selectivity of the target product,with the best yield of 54.8%.The intermediate N-ethyl-2-methylpyrrolidine was separated by vacuum distillation,and this new compound was confirmed by GC-MS and NMR.（2）Ammoxidation of N-ethyl-2-methylpyrrolidine on the VOx@Ti O₂catalyst was investigated.Three Ti O₂supports were prepared by doped with high clay or alumina,and the corresponding catalysts were prepared after vanadium loading through crystallization.It was showed that the crystallized catalyst was different from the crystal phase of the support by characterization of XRD,NH₃-TPD,O₂-TPD and BET.After Vanadium loading,the conversion of Ti O₂from anatase to rutile was promoted,and the surface acidity decreased significantly.The model reaction of ammoxidation of toluene to benzonitrile was used.It was found that the pore size and surface acidity of the catalyst were increased on VOx@Ti O₂doped by alumina,with the obviously improving yield.The catalyst was initially applied to the ammoxidation of N-ethyl-2-methylpyrrolidine with the yield of 81.3 mole%.（3）The catalytic performance of Raney nickel catalyst for the hydrogenation of nitriles was investigated.Raney nickel was used as catalyst and benzonitrile as model reaction.The effects of solvent,Na OH content,reaction pressure and reaction temperature were investigated.Under the optimum conditions,the selectivity of benzylamine was up to 92.4 mole%...