Potassium Hydroxide → HCID 90103465, Verbindung

Temperatur

0 °C

In a 100 mL round-bottomed flask, KOH (356 mg, 5.45 mmol) was combined with H2O (50 ml) to give a colorless solution and cooled to 0° C. 4,4,4-Trifluoro-3-nitromethyl-butyric acid ethyl ester (1.25 g, 5.45 mmol) in 10 ml THF was added and the resulting reaction mixture was stirred for 20 min. This was followed by addition of MgSO4 (657 mg, 5.45 mmol) in 5 ml of H2O then by KMnO4 (862 mg, 5.45 mmol) in 30 ml of H2O. The resulting reaction mixture was stirred for 30 min, filtered through celite and the celite cake washed with CH2Cl2. The combined filtrate and washes were washed with brine, dried over Na2SO4, filtered and concentrated to afford 4,4,4-trifluoro-3-formyl-butyric acid ethyl ester as a liquid which was used without purification.

1. customto give a colorless solution
2. customthe resulting reaction mixture
3. customThe resulting reaction mixture
4. stirringwas stirred for 30 min
5. filtrationfiltered through celite
6. washthe celite cake washed with CH2Cl2
7. washThe combined filtrate and washes were washed with brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated

ORD-Eintrag

ord-955962637e704064a17b9764098c1f08

Quelldatensatz

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09388172B2