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0 °C

4-Bromo-2-(cyanomethyl)benzonitrile (75 g, 339 mmol) was added to 2,2-dichloroacetic acid (150 mL, 339 mmol). The resulting solution was cooled to 0° C. in an ice-water bath. HBr (27.5 g, 339 mmol) was bubbled through the cold solution until a yellow precipitate crashed out of solution, resulting in a yellow slurry. HBr was bubbled through the slurry for an additional 5 minutes. The solution was allowed to warm to room temperature over 1 hour. The slurry was then cooled to 0° C. in an ice-water bath and diethyl ether (200 mL) was added. The mixture was stirred for 20 minutes at 5° C. The product was recovered as a yellow solid by filtration (42 g, 41%). LCMS (API-ES) m/z: 303 (M+H+).

1. customresulting in a yellow slurry
2. customHBr was bubbled through the slurry for an additional 5 minutes
3. temperatureto warm to room temperature over 1 hour
4. temperatureThe slurry was then cooled to 0° C. in an ice-water bath
5. additiondiethyl ether (200 mL) was added
6. filtrationThe product was recovered as a yellow solid by filtration (42 g, 41%)