反应详情

温度

60 °C

To a 3 L round bottom flask were added 6-tert-butyl-8-fluoro-2H-phthalazin-1-one (132.3 g, 0.6 mol), 2-chloro-6-fluorobenzaldehyde (104.8 g, 0.66 mol) and cesium carbonate (117.4 g, 0.36 mol). The flask was evacuated and backfilled with Nitrogen three times. Then, ethoxytrimethylsilane (142 g, 1.2 mol) and DMF (1.6 L) were added to the reaction flask, and the resulting mixture was heated to 60° C. After 4 h stirring, the solution was allowed to cool down to ambient temperature and the reaction was quenched by addition of 800 mL of H2O dropwise. The desired product started to precipitate from DMF and water mixture. The solid was collected by filtration after cooling down to 5° C., and washed with DMF/water (2/1, 750 mL, pre-cooled to 6° C.) and H2O (400 mL). The filter cake was dried under vacuum oven at 65° C. overnight to afford 147 g of the title compound (68.2% isolated yield) as a yellow solid. MS (ESI) 358, 360 (M+H)−.

1. customThe flask was evacuated
2. temperatureto cool down to ambient temperature
3. customthe reaction was quenched by addition of 800 mL of H2O dropwise
4. customto precipitate from DMF and water mixture
5. filtrationThe solid was collected by filtration
6. temperatureafter cooling down to 5° C.
7. washwashed with DMF/water (2/1, 750 mL, pre-cooled to 6° C.) and H2O (400 mL)
8. customThe filter cake was dried under vacuum oven at 65° C. overnight