Ethanol → Ethyl 2-fluoroethyl carbonate

Temperature

-78 °C

In a 100 mL PFA-flask fluoroethyl fluoroformate (27.0 g, 245 mmol) was added to dry NaF (15 g; 357 mmol). After cooling the mixture to −78° C. ethanol (12 mL, 310 mmol) was added over a period of 15 min. The mixture was stirred at −78° C. for 30 min. After warming up to room temperature the reaction was stirred for further 16 h. After addition of 5 g molecular sieve (0.4 nm) and stirring for 4 h at room temperature, all solids were removed by filtration and the resulting crude product was purified by distillation under reduced pressure (100 mbar).

1. additionwas added over a period of 15 min
2. temperatureAfter warming up to room temperature the reaction
3. stirringwas stirred for further 16 h
4. additionAfter addition of 5 g molecular sieve (0.4 nm)
5. stirringstirring for 4 h at room temperature
6. customall solids were removed by filtration
7. distillationthe resulting crude product was purified by distillation under reduced pressure (100 mbar)

ORD record

ord-8162fa4003034bf284fdfd24631e0e71

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09000204B2