反应详情

温度

120 °C

DMA (60 ml) and potassium carbonate (5.65 g, 40.86 mmol) were added to the flask containing 4-fluoro-2-methoxy-1-nitrobenzene (1.748 g, 10.22 mmol) and (3R,4S)—N-benzyl-3-fluoropiperidin-4-amine HCl salt (INTERMEDIATE 46, 2.5 g, 10.22 mmol). The reaction was heated to 120° C. for 5 h. The reaction mixture was cooled to rt, and filtered. The filtrate was diluted with EtOAc (50 ml) and the solution was washed with brine (2×100 ml). The organic layer was dried over Na2SO4, filtered, and concentrated to give a crude yellow liquid. It was purified using silica gel chromatography (80-100% EtOAc/hexane) to give the title product (2.200 g, 59.9%). m/z 361.

1. temperatureThe reaction mixture was cooled to rt
2. filtrationfiltered
3. additionThe filtrate was diluted with EtOAc (50 ml)
4. washthe solution was washed with brine (2×100 ml)
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a crude yellow liquid
9. customIt was purified