反应详情

温度

65 °C

To a mixture of 5-(4-chlorobenzyl)-6-(3-chlorophenyl)-3-(3-hydroxypropyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione (22.25 mg, 0.05 mmol), K2CO3 (13.8 mg, 0.1 mmol) in DMF (1 mL) was added CH3I (8.5 mg, 0.06 mmol). The reaction was heated in a sealed tube at 65° C. for 2 h, cooled to RT then diluted with EA (10 mL) and water (3 mL). The organic layer was washed with brine (3 mL) dried over Na2SO4 and concentrated to a residue which was purified by Prep HPLC to give 5-(4-chlorobenzyl)-6-(3-chlorophenyl)-3-(3-hydroxypropyl)-1-methylfuro[2,3-d]pyrimidine-2,4(1H,3H)-dione (3 mg, 13% yield) as a white solid. 1H NMR (DMSO-d6) δ: 7.62 (s, 1H), 7.54 (d, J=8.0 Hz, 1H), 7.47 (t, J=7.9 Hz, 1H), 7.41 (d, J=8.0 Hz, 1H), 7.35 (d, J=8.5 Hz, 2H), 7.26 (d, J=8.5 Hz, 2H), 4.47 (t, J=5.2 Hz, 1H), 4.32 (s, 2H), 3.97-3.81 (m, 2H), 3.53 (s, 3H), 3.43 (dd, J=11.8, 6.4 Hz, 2H), 1.75-1.60 (m, 2H). LCMS: MH+ 459 and TR=3.047 min.

1. temperaturecooled to RT
2. washThe organic layer was washed with brine (3 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated to a residue which
5. customwas purified by Prep HPLC