反应详情

温度

120 °C

A microwave vial equipped with a magnetic stirrer was charged with 296c (2.67 g, 10.0 mmol), 2-methoxyethanamine (2.25 g, 30.0 mmol), and DMSO (14 mL). The reaction mixture was heated at 120° C. under microwave irradiation for 1.0 h. It was cooled to room temperature and diluted with ethyl acetate (40 mL). The mixture was washed with water (3×15 mL). The organic layer was dried and filtered. The filtrate was concentrated under pressure and the residual was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 296d (1.7 g, 75%) as a yellow solid. MS-ESI: [M+H]+ 227.0

1. customA microwave vial equipped with a magnetic stirrer
2. temperatureIt was cooled to room temperature
3. washThe mixture was washed with water (3×15 mL)
4. customThe organic layer was dried
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under pressure
7. customthe residual was purified by silica-gel column chromatography
8. washeluting with 30:1 dichloromethane/methanol