反应详情

A solution of potassium hydroxide (13.08 g, 233 mmol) in water (25.2 mL) was added slowly to a solution of 5-bromo-1H-indole-2,3-dione (9.76 g, 38.9 mmol) in ethanol (63.1 mL). 1-[4-(trifluoromethyl)phenyl]-1-propanone (8.64 g, 42.7 mmol) was added and the mixture was heated to reflux for 1 h. The reaction mixture was concentrated to remove the solvent, the residue was dissolved in water, and the mixture was washed three times with Et2O. The aqueous mixture was chilled, and concentrated HCl was added until the solution was pH 3. The solid was collected by filtration, washed with water, and dried under reduced pressure in a water bath at 100° C. The product was obtained as a light brown powder (15.6 g, 98%). This material was used without further purification. MS (m/z) 412.0 (M+H+).

1. temperaturethe mixture was heated
2. temperatureto reflux for 1 h
3. concentrationThe reaction mixture was concentrated
4. customto remove the solvent
5. dissolutionthe residue was dissolved in water
6. washthe mixture was washed three times with Et2O
7. temperatureThe aqueous mixture was chilled
8. additionconcentrated HCl was added until the solution
9. filtrationThe solid was collected by filtration
10. washwashed with water
11. customdried under reduced pressure in a water bath at 100° C