反应详情

To a stirred solution of 3,5-bis(trifluoromethyl)acetophenone (50.0 g, 195.2 mmol) in acetic acid (200 mL) was added dropwise at 90° C. bromine (31.2 g, 195.2 mmol). After the initiation of the reaction (3-4 drops), the oil bath was removed and the mixture was stirred at room temperature for 1 h. To this mixture was added water (50 mL) and the mixture was concentrated under reduced pressure. The resulting residue was partitioned between ethyl acetate (500 mL) and water (500 mL). The organic layer was separated and washed with saturated sodium hydrogen carbonate (250 mL×2), and saturated sodium chloride (250 mL), dried (MgSO4), filtered and concentrated under reduced pressure to give 1-[3,5-bis(trifluoromethyl)phenyl]-2-bromoethanone (57.65 g, 88%) as a colorless solid.

1. customAfter the initiation of the reaction (3-4 drops)
2. customthe oil bath was removed
3. additionTo this mixture was added water (50 mL)
4. concentrationthe mixture was concentrated under reduced pressure
5. customThe resulting residue was partitioned between ethyl acetate (500 mL) and water (500 mL)
6. customThe organic layer was separated
7. washwashed with saturated sodium hydrogen carbonate (250 mL×2), and saturated sodium chloride (250 mL)
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure