反应详情

温度

90 °C

Potassium carbonate (2.3 g, 16.7 mmol) was added to a solution of example 6a (5.1 g, 23.8 mmol) in DMF (20 mL). The reaction mixture was stirred at 90° C. for 1 h. Chloroacetone (2.21 g, 23.8 mmol) was then added dropwise at room temperature and the reaction mixture was heated at 55° C. for 1.5 h. The reaction mixture was poured into ice. The precipitate was collected by filtration to give 6.53 g (quantitative) of the title compound as an off-white solid. 1H NMR (400 MHz, DMSO-d6): δ 7.66 (s, 1H), 6.69 (dd, 1H, J=12.0, 1.2 Hz), 6.49 (dt, 1H, J=12.0, 1.2 Hz), 5.02 (s, 2H), 3.34-3.40 (m, 1H), 2.15 (s, 3H), 0.81-0.85 (m, 2H), 0.48-0.52 (m, 2H). MS (ES) [m+H] calc'd for C13H13F2NO3, 269; found 269.

1. temperaturethe reaction mixture was heated at 55° C. for 1.5 h
2. additionThe reaction mixture was poured into ice
3. filtrationThe precipitate was collected by filtration