Ethanol → HCID 86668093, compound

Crude 3-fluoro-2-fluoromethyl-2-hydroxy-propionic acid (17 g) was dissolved in ethanol (400 ml) and H2SO4 (98%, 30 g) was added. The reaction mixture was refluxed for 16 h. The reaction mixture was cooled to ambient temperature and filtered. The solution was carefully treated with 30 g solid Na2CO3 and the resulting mixture was stirred for 30 min at room temperature. 400 ml DCM were added and the mixture was filtered. The solution was concentrated (50° C., 150 mbar) and further purified by distillation (82° C., 20 mbar) to give a colorless liquid.

1. temperatureThe reaction mixture was refluxed for 16 h
2. filtrationfiltered
3. additionThe solution was carefully treated with 30 g solid Na2CO3
4. addition400 ml DCM were added
5. filtrationthe mixture was filtered
6. concentrationThe solution was concentrated (50° C., 150 mbar)
7. distillationfurther purified by distillation (82° C., 20 mbar)
8. customto give a colorless liquid

ORD record

ord-f81e3bc5dc6943a7b383b0bd4314190f

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08865712B2