反应详情

(3-Bromo-5-(trifluoromethyl)phenyl)methanol (1.4 g, 5.5 mmol), tetrakis(triphenylphosphine) palladium(0) (0.64, 0.55 mmol) and zinc cyanide (388 mg, 3.31 mmol) were combined in dimethylformamide (6 mL). The reaction mixture degassed repeatedly using the freeze-thaw method. After warming to room temperature, the reaction was heated at 90° C. for 1 h, cooled to room temperature and concentrated. The crude product was dissolved in ethyl acetate, washed with water (2×), 1 N hydrochloric acid (2×), brine (2×), dried over sodium sulfate, and concentrated. Flash chromatography on silica gel gave 0.37 g (33%). LC/MS (HPLC method 3): tR=2.06 min, 202.02 (MH)+.

1. customThe reaction mixture degassed repeatedly
2. temperaturethe reaction was heated at 90° C. for 1 h
3. temperaturecooled to room temperature
4. concentrationconcentrated
5. dissolutionThe crude product was dissolved in ethyl acetate
6. washwashed with water (2×), 1 N hydrochloric acid (2×), brine (2×)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customFlash chromatography on silica gel gave 0.37 g (33%)