反应详情

温度

50 °C

A sealed suspension of 3-hydroxy-1-methypyridin-4(1H)-one (1.00 g, 8.0 mmol) and potassium carbonate (0.11 g, 0.8 mmol) in 2.4 mL of difluoroacetaldehyde ethyl hemiacetal was heated to 50° C. for 18 h. The volatile components were evaporated under reduced pressure. The residue was dissolved in 3 mL of de-ionized water then cooled in an ice-water bath, and the pH was adjusted to 5-6 with a 1N HCl solution. The precipitate was collected by suction filtration and dried. Thus, the title compound Apo7078 was obtained (410 mg) as a white solid. Yield=25%; 1H NMR (400 MHz, CD3OD) δ (ppm): 7.62 (d, J=7.1 Hz, 1H), 6.41 (d, J=7.1 Hz, 1H), 6.30 (dt, 3J=55.8 Hz, 2J=5.1 Hz, 1H), 5.45 (dt, 2J=5.1 Hz, 3J=11.4 Hz, 1H), 3.96 (s, 3H); MS m/z 206 [M+1], 188 (100%).

1. customThe volatile components were evaporated under reduced pressure
2. dissolutionThe residue was dissolved in 3 mL of de-ionized water
3. temperaturethen cooled in an ice-water bath
4. filtrationThe precipitate was collected by suction filtration
5. customdried