反应详情

温度

-60 °C

To a solution of methyl 3-(6-bromo-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propanoate (5.1 g, 14.96 mmol) in THF (500 mL) at −60° C., was added diisobutylaluminium hydride (1.5 M in toluene, 40 mL, 60 mmol) dropwise. The reaction was stirred at −60° C. for 3 h, warmed to 0° C., quenched with aq. NH4Cl (150 mL) then extracted with EA (200 mL). The organic layer was washed with brine (100 mL), dried over Na2SO4 and concentrated to give 6-bromo-3-(3-hydroxypropyl)-1-methylpyrido[2,3-d]pyrimidine-2,4 (1H,3H)-dione (6.2 g, >100% yield) as a yellow oil. LCMS: MH+ 314 and TR=0.882 min. Used without further purification.

1. temperaturewarmed to 0° C.
2. customquenched with aq. NH4Cl (150 mL)
3. extractionthen extracted with EA (200 mL)
4. washThe organic layer was washed with brine (100 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated