Synthesis
General procedure for the synthesis of ethyl 3-oxo-3-hydrazinopropionate from diethyl malonate: diethyl malonate (10 g, 62.5 mmol) was dissolved in 50 ml of anhydrous ethanol, followed by slow addition of 85% hydrazine hydrate (1.44 g, 1.44 mol). The reaction mixture was stirred and reacted at room temperature overnight. After completion of the reaction, filtration was carried out and the filtrate was collected. The solvent was removed by distillation under reduced pressure to give the crude product. The crude product was purified by recrystallization with a mixed solvent of ethyl acetate/petroleum ether to finally obtain the target compound ethyl 3-oxo-3-hydrazinopropionate (2.10 g, 64% yield) as a white solid.
References
[1] Patent: CN107629014, 2018, A. Location in patent: Paragraph 0016; 0017
[2] European Journal of Medicinal Chemistry, 2008, vol. 43, # 3, p. 584 - 594
[3] Liebigs Annalen der Chemie, 1990, # 9, p. 841 - 846
[4] European Journal of Medicinal Chemistry, 2013, vol. 70, p. 358 - 363
[5] Chinese Chemical Letters, 2017, vol. 28, # 5, p. 1031 - 1034
