反应详情

温度

65 °C

To a mixture of 6-bromo-1-methyl-2,4-dioxo-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-5-carbaldehyde (100 mg, 0.23 mmol), K2CO3 (159 mg, 1.15 mmol) in DMF (3 mL) was added 3-chlorophenol (90 mg, 0.70 mmol). The reaction was heated at 65° C. for 1 h, cooled to RT then diluted with EA (30 mL) and water (30 mL). The organic layer was dried over Na2SO4 and concentrated to a residue which was purified by chromatography and eluted with PE/EA (5:1) to give 6-(3-chlorophenoxy)-1-methyl-2,4-dioxo-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-5-carbaldehyde (65 mg, 58.6% yield) as a yellow oil. LCMS: MH+ 479 and TR=1.836 min.

1. temperaturecooled to RT
2. dry with materialThe organic layer was dried over Na2SO4
3. concentrationconcentrated to a residue which
4. customwas purified by chromatography
5. washeluted with PE/EA (5:1)