反应详情

温度

60 °C

A mixture of ethyl 5-(benzyloxy)-1-(methylsulfonyl)-2-(4-((methylsulfonyloxy)methyl)piperidin-1-yl)-6-oxo-1,6-dihydropyrimidine-4-carboxylate and K2CO3 (0.051 g, 0.368 mmol) in ethanol (10 mL) was stirred at 60° C. for 4 h and cooled to room temperature. Water was added and the product was extracted with ethyl acetate. The organic phase was washed with brine then dried (Na2SO4), filtered and concentrated. The residue was purified by flash column chromatography (Biotage flash chromatography system; 0%-10% methanol/CH2Cl2, 25 CV; 10% methanol/CH2Cl2, 5 CV) to give the title compound as a white glass (0.0248 g, 37% yield). 1H NMR (500 MHz, CDCl3) δ: 7.44 (2H, dd, J=7.3 Hz), 7.30-7.22 (3H, m), 5.27 (2H, s), 4.22 (2H, q, J=7.1 Hz), 4.01-3.94 (2H, m), 3.77-3.70 (2H, m), 3.67 (2H, brs), 3.02 (1H, brs), 2.29-2.24 (2H, m), 1.93-1.88 (2H, m), 1.22 (3H, t, J=7.0 Hz). LCMS (M+H) calcd for C20H24N3O4: 370.17; found: 370.30.

1. temperaturecooled to room temperature
2. extractionthe product was extracted with ethyl acetate
3. washThe organic phase was washed with brine
4. dry with materialthen dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by flash column chromatography (Biotage flash chromatography system; 0%-10% methanol/CH2Cl2, 25 CV; 10% methanol/CH2Cl2, 5 CV)