反应详情

温度

125 °C

tert-Butyl 2-(3-cyano-4-fluorophenyl)acetate (2.0 g, 8.5 mmol) and the product of step A (2.9 g, 10 mmol) were diluted with DMSO (22 mL) followed by the addition of potassium carbonate (1.4 g, 10 mmol). The reaction was heated to 125° C. and stirred for 12 hours. The reaction mixture was then cooled to room temperature, diluted with ethyl acetate and 10% aqueous sodium carbonate. The layers were separated and the organic layer was washed with 10% aqueous sodium carbonate two more times followed by water and brine. The organic material was dried over MgSO4, filtered and concentrated. The material was purified using a biotage 40M column eluting with hexanes:ethyl acetate (8:2) to yield tert-butyl 2-(3-cyano-4-(4-(3,4-dichlorobenzamido)phenoxy)phenyl)acetate (2.5 g, 59% yield) as a white solid.

1. temperatureThe reaction mixture was then cooled to room temperature
2. customThe layers were separated
3. washthe organic layer was washed with 10% aqueous sodium carbonate two more times
4. dry with materialThe organic material was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe material was purified
8. washeluting with hexanes:ethyl acetate (8:2)