反应详情

To a solution of ethyl 3-(1,5-dimethyl-2,4-dioxo-6-(3-(trifluoromethoxy)phenyl)-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoate (120 mg, 0.22 mmol) in CCl4 (3 mL) was added NBS (39 mg, 0.22 mmol) followed by benzoyl peroxide (5 mg). The reaction was heated at reflux for 4 h, cooled to RT and diluted with DCM (10 mL). The mixture was washed with aq. NaHCO3 (10 mL), and brine (10 mL). The organic layer was dried over Na2SO4 and concentrated to give ethyl 3-(5-(bromomethyl)-1-methyl-2,4-dioxo-6-(3-(trifluoromethoxy)phenyl)-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoate (100 mg, 85.7% yield) as an oil. LCMS: MH+ 535 and TR=2.087 min. Used without further purification.

1. temperatureThe reaction was heated
2. temperatureat reflux for 4 h
3. washThe mixture was washed with aq. NaHCO3 (10 mL), and brine (10 mL)
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated