反应详情

温度

40 °C

To a solution of 3-(5-methyl-2,4-dioxo-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoic acid (330 mg, 1.17 mmol) in DMF (6 mL) was added CH3I (332 mg, 2.33 mmol) followed by K2CO3 (322 mg, 2.33 mmol). The reaction was heated in a sealed tube at 40° C. for 4 h, cooled to RT then diluted with EA (20 mL) and water (20 mL). The organic layer was washed with brine (10 mL), dried over Na2SO4 and concentrated to a residue which was purified by chromatography eluted with DCM/MeOH (50:1) to give methyl 3-(1,5-dimethyl-2,4-dioxo-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoate (210 mg, 63.6% yield) as a yellow solid. LCMS: MH+ 283 and TR=1.253 min.

1. temperaturecooled to RT
2. washThe organic layer was washed with brine (10 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated to a residue which
5. customwas purified by chromatography
6. washeluted with DCM/MeOH (50:1)