反应详情

温度

40 °C

To a solution of 5-bromo-2-(3-(3-methoxy-3-oxopropyl)ureido)nicotinic acid (15 g, 43.5 mmol) in acetone (150 mL) was added K2CO3 (18 g, 130.4 mmol) followed by CH3I (18 mL, 263.1 mmol). The reaction was heated in a sealed flask at 40° C. for 24 h, cooled to RT, concentrated then diluted with EA (200 mL) and water (100 ml). The organic layer was washed with brine (100 mL), dried over Na2SO4, filtered and concentrated to a residue which was purified by chromatography PE/EA eluted with (10:1 to 2:1) to give methyl 3-(6-bromo-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propanoate (5.1 g, 34.4% yield) as a white solid. LCMS: MH+ 342 and TR=1.266 min. Used without further purification.

1. temperaturecooled to RT
2. concentrationconcentrated
3. additionthen diluted with EA (200 mL) and water (100 ml)
4. washThe organic layer was washed with brine (100 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated to a residue which
8. customwas purified by chromatography PE/EA
9. washeluted with (10:1 to 2:1)