反应详情

温度

150 °C

A mixture of N-(2-oxo-2-phenylethyl)-4-(phenylmethyl)-2-morpholinecarboxamide (850 mg, 2.51 mmol) and ammonium trifluoroacetate (1317 mg, 10.05 mmol) was heated at 150° C. under microwave condition with stirring for 1 hour. Water (150 mL) was added to the residue, and extracted with EtOAc (200 mL). The organic layer was dried (Na2SO4), filtered, and concentrated to afford the crude title compound (1.3 g) as a brown oil. This material was combined with another batch of crude title compound (250 mg) and purified by silica gel chromatography using as eluent EtOAc (1600 mL) in hexanes (400 mL) to afford the title compound (900 mg, 2.82 mmol) as a brown solid. LC-MS (ES) m/z=320 [M+H]+.

1. extractionextracted with EtOAc (200 mL)
2. dry with materialThe organic layer was dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto afford the crude title compound (1.3 g) as a brown oil
6. custompurified by silica gel chromatography