Cesium carbonate → HCID 57633709, Verbindung

Temperatur

120 °C

To a solution of 4-amino-2-(trifluoromethyl)benzonitrile (0.100 g, 0.54 mmol) in acetonitrile (3 mL) was added cesium carbonate (0.438 g, 1.34 mmol) and 1-bromo-2-fluoroethane (0.340 g, 2.68 mmol). The mixture was heated in a microwave at 120° C. for 15 min. Upon cooling, additional 1-bromo-2-fluoroethane (0.340 g, 2.68 mmol) was added and the reaction was heated in the microwave at 140° C. for 20 min. Upon cooling, the solids were filtered off and washed with ethyl acetate. The filtrate was concentrated in vacuo and the residue was purified by radial chromatography (10-40% ethyl acetate-hexane gradient) to give 0.100 g of a mixture (6:1) of the title compound and 4-[bis(2-fluoroethyl)amino]-2-(trifluoromethyl)benzonitrile as a white solid, which was used as such in the next reaction.

1. temperatureUpon cooling
2. temperaturethe reaction was heated in the microwave at 140° C. for 20 min
3. temperatureUpon cooling
4. filtrationthe solids were filtered off
5. washwashed with ethyl acetate
6. concentrationThe filtrate was concentrated in vacuo
7. customthe residue was purified by radial chromatography (10-40% ethyl acetate-hexane gradient)

ORD-Eintrag

ord-90416fac95e74e16af449b2d5c69ff5e

Quelldatensatz

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07723385B2