Chlorodifluoroacetic acid ethyl ester

64-17-5

76-04-0

383-62-0

General procedure for the synthesis of ethyl difluorochloroacetate from ethanol and difluorochloroacetic acid: 504.3 g (3.87 mmol) of difluorochloroacetic acid and 5.0 g of p-toluenesulfonic acid were dissolved in 775 mL of dichloromethane, and 311.6 g (6.76 mol) of ethanol was slowly added over a 30-minute period at room temperature (the temperature was raised to 33 °C during the reaction). The mixture was assembled to a water condenser and stirred at reflux for 38 hours and then cooled to room temperature. The reaction mixture was washed sequentially with 200 mL of water, 200 mL of saturated sodium bicarbonate solution and 200 mL of water, followed by drying with anhydrous sodium sulfate, filtration and distillation. Further purification by fractional distillation afforded 488.9 g (98% purity, 78.5% yield) of ethyl difluorochloroacetate with a boiling point of 94-96 °C.