Diethyl aminomalonate (17.5 g, 0.1 mol) and triethylamine (20 g, 0.2 mol) were dissolved in 250 mL of dichloromethane in a three-necked flask under ice bath conditions. Subsequently, di-tert-butyl dicarbonate (26 g, 0.12 mol) was slowly added. The reaction mixture was gradually brought to room temperature and stirred continuously at this temperature and the progress of the reaction was monitored by thin layer chromatography (TLC). After completion of the reaction, the solvent was removed by distillation under reduced pressure. The residue was extracted with dichloromethane (200 mL × 3). The organic phases were combined, dried with anhydrous magnesium sulfate, and concentrated to give 27 g of the colorless oily product diethyl 2-Boc-aminomalonate in 98% yield.
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