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0 °C

1.60 g (14 mmol) of t-butoxypotassium was added to a solution prepared by dissolving 20.30 g (0.1 mol) of ethyl 2-bromo-2,2-difluoroacetate in 140 ml of benzyl alcohol and 1200 ml of hexane at 0° C. in a nitrogen atmosphere. The mixture was stirred at 0° C. for 1 hour. After confirming disappearance of the raw materials by thin-layer chromatography (TLC), the reaction was terminated by adding 120 ml of concentrated hydrochloric acid. The mixture was washed twice with water, washed twice with a saturated sodium chloride solution, and dried over anhydrous sodium sulfate. After evaporating the solvent under reduced pressure, the product was purified by column chromatography to obtain 15.37 g of benzyl 2-bromo-2,2-difluoroacetate shown by the following formula (yield: 58%).

1. customprepared
2. customthe reaction was terminated
3. additionby adding 120 ml of concentrated hydrochloric acid
4. washThe mixture was washed twice with water
5. washwashed twice with a saturated sodium chloride solution
6. dry with materialdried over anhydrous sodium sulfate
7. customAfter evaporating the solvent under reduced pressure
8. customthe product was purified by column chromatography