Methanol → 3,3,3-Trifluoro-2-oxopropanoic acid

To a solution of ethyl 3,3,3-trifluoro-2-oxopropanoate (5 g, 29.36 mmol) in ethanol (30 ml) was slowly added aqueous sodium hydroxide ((2.35 g, 58.72 mmol, dissolved in water (30 ml)), and stirred for 20 h at room temperature until the starting material was consumed. The reaction mixture was concentrated and the resulting white solid was dissolved in water (100 ml). The aqueous layer was extracted by ethyl acetate (50 ml×2), and then the aqueous layer was adjusted PH to 1˜2 with concentrated HCl, and concentrated to give a white solid. The solid was added to methanol (200 ml) and stirred for overnight, filtered, and the filtrate was concentrated and dried to give the crude product (4.13 g, 99%) as a white solid, used in next step without further purification.

1. customwas consumed
2. concentrationThe reaction mixture was concentrated
3. dissolutionthe resulting white solid was dissolved in water (100 ml)
4. extractionThe aqueous layer was extracted by ethyl acetate (50 ml×2)
5. concentrationconcentrated
6. customto give a white solid
7. stirringstirred for overnight
8. filtrationfiltered
9. concentrationthe filtrate was concentrated
10. customdried

ORD-Eintrag

ord-27f5700531104a47b23d5f85784dd2b2

Quelldatensatz

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08999985B2