Synthesis And Characterization Of Ethy 4-Amino-1-piperidinecarboxylate

An important product Ethy 4-Amino-1-piperidinecarboxylate was synthesized using 1-(Benzyloxycarbonyl)-4-piperidinone as initial material through preparing of 4-Piperidone hydrate hydrochloride, Ethyl 4-oxo-l-piperidinecarboxylate and 4-hydroxyimino Amino-1-ethyl piperidine. All products were characterized by IR,'HNMR, MS and so on.Effect of the reaction temperature, reaction time, material ratio, dosage of catalyst was studied mainly through single factor experiment. The optimum reaction conditions were obtained. The yield of 4-Piperidone hydrate hydrochloride was 97.5% when the mole ratio of material was 5.28:6, reaction temperature was 25℃, reaction pressure was 4 atm and reaction time was 24h. A 97.3% yield of Ethyl 4-oxo-l-piperidinecarboxylate was obtained when the mole ratio of material was 10:1, the alkali of acid was 2:1, reaction temperature was 0℃and reaction time was 20min. The yield of 4-hydroxyimino amino-1-ethyl piperidine was 95.4% when the mole ratio of material was 1:1, reaction temperature was 25℃and reaction time was 24h, then a 91.2% yield of Ethy 4-amino-l-piperidinecarboxylate was obtained while the mole ratio of material was 1:1 and reaction temperature was 60℃。Besides, a 92% yield of Ethy 4-amino-l-piperidinecarboxylate was also obtained when the mole ratio of material was 5:2:1, reaction temperature was 25℃and reaction time was 6h; and then the mole ratio of material was 1.5:1, reaction temperature was 25℃and reaction time was 3h。...