Trichloroacetyl chloride → Methyl triflate

Temperature

90 °C

17.74 g (0.1182 mol) of trifluoromethanesulfonic acid are introduced into a round-bottomed flask fitted with a reflux condenser. 21.41 g (0.1177 mol) of trichloroacetyl chloride are added over the course of 2 minutes with constant stirring. 10.60 g (0.1177 mol) of dimethyl carbonate are then added over the course of 5 minutes without cooling the mixture. The reaction mixture warms slightly and is heated at 80-100° C. for 7 hours in an oil bath (temperature in the oil bath) with stirring until the evolution of gas ceases. After cooling to room temperature, the mixture is distilled under atmospheric pressure, giving 17.48 g (yield: 90.5%) of methyl trifluoromethanesulfonate as a transparent, colourless liquid (boiling range 98-100° C.).

1. customfitted with a reflux condenser
2. temperaturewithout cooling the mixture
3. temperatureAfter cooling to room temperature
4. distillationthe mixture is distilled under atmospheric pressure

ORD record

ord-795d2de737564d13a07a4b927284ff40

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07247740B2