Nitric Acid → HCID 178526837, Verbindung

Temperatur

0 °C

3-(Trifluoromethyl)pyridin-2-ol (2.3 g) was added to concentrated sulfuric acid (15 mL) at 0° C. The mixture was stirred at 0° C. for 5 minutes. To this solution was added fuming nitric acid (6 mL) dropwise over 5 minutes. The reaction mixture was stirred at room temperature for 2 hours, and then heated at 50° C. for 3 hours. After cooling, the reaction mixture was poured onto ice (200 g), and the mixture was extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure to provide the title compound.

1. stirringThe reaction mixture was stirred at room temperature for 2 hours
2. temperatureheated at 50° C. for 3 hours
3. temperatureAfter cooling
4. additionthe reaction mixture was poured onto ice (200 g)
5. extractionthe mixture was extracted with ethyl acetate three times
6. washThe combined organic layers were washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-dda35ac380954eff9314af5a57f566c9

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09034875B2