反应详情

A mixture of 6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-1-[2-fluoro-6-(4-methoxy-benzylamino)-pyridin-4-ylmethyl]-5-isopropyl-1H-pyrimidine-2,4-dione (714 mg, 1.24 mmol), PPTS (62 mg, 0.25 mmol), and water (5 drops) in acetone (10 ml) was heated under reflux for 3 hr. After cooling to room temperature, the mixture was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA: hexanes (from 1:1 to 2:3)) to afford 548 mg (83%) of a white solid. 1H NMR (200 MHz, CD3OD/CDCl3) δ 1.00 (6H, d, J=7.4 Hz), 2.30 (3H, s), 2.58 (1H, m), 3.71 (3H, s), 4.19 (2H, s), 4.65 (2H, s), 5.78 (1H, s), 5.86 (1H, s), 6.76-6.80 (3H, m), 7.02 (1H, s), 7.11-7.16 (2H, s), 7.32 (1H, s), 9.78 (1H, s).

1. temperaturewas heated
2. temperatureunder reflux for 3 hr
3. customthe mixture was evaporated in vacuo
4. customthe residue was purified by silica gel column chromatography (eluent, EA: hexanes (from 1:1 to 2:3))