1260672-03-4

94193-77-8

1260672-03-4

General procedure for the synthesis of 5-phenylmorpholin-3-one from the compound (CAS:94193-77-8): crude 2-chloro-N-(2-hydroxy-1-phenylethyl)acetamide (3 g, 14.04 mmol) was dissolved in anhydrous tetrahydrofuran (THF, 40 mL) and the reaction mixture was cooled to 0 °C. Sodium hydride (NaH, 0.842 g, 35.1 mmol) was added in two portions, followed by slow warming of the reaction mixture to room temperature. Upon completion of the reaction, the reaction was quenched by slow addition of 50% THF/water solution followed by dilution with ethyl acetate (EtOAc). The organic layer was washed sequentially with aqueous sodium bicarbonate (NaHCO3), water and brine. The organic phases were combined and purified by fast column chromatography (eluent: 30-100% EtOAc/heptane gradient) to afford the target product 5-phenylmorpholin-3-one (2.25 g, 90% yield). Liquid chromatography-mass spectrometry (LC/MS) analysis showed the following results: retention time (Rt) = 0.39 min (Table 1, method f); mass spectrum (MS) m/z: 219 ([M+H+MeCN]+).